JP5416348B2 - Gas generation reactor having solid-gas separation function - Google Patents

Description

  The present invention relates to a gas generation reaction apparatus having a solid-gas separation function used in a coolant waste liquid treatment apparatus used for cutting a silicon wafer, and more specifically, a gas generated by a reaction between a metal component and an alkali, Solid-gas separation that prevents the interference with the residual solids settled after the reaction, enables continuous processing while efficiently discharging the solids after the reaction to the outside of the system, and allows the entire device to be compactly formed. The present invention relates to a gas generating reaction device having a function.

  For example, when a silicon wafer is manufactured by cutting a single crystal ingot with a multi-wire saw, a coolant in which abrasive grains are dispersed is used as a grinding liquid. The coolant is regenerated from the used grinding fluid waste, and abrasive grains such as silicon carbide are recovered. However, since this grinding waste contains silicon grinding powder, it is necessary to remove the silicon particles. There is. Also, the waste after recovering coolant and abrasive grains from the grinding waste liquid may cause hydrogen gas to react with the water contained in the metal silicon contained therein. When this is discarded, the metal silicon is harmless. It is necessary to make it.

  Conventionally, as a method of removing silicon particles from the above grinding waste liquid, a method of dissolving in an alkali has been proposed (see, for example, Patent Documents 1 and 2). That is, in these prior arts, the grinding waste liquid and the alkaline aqueous solution are charged into the reaction chamber in the reaction vessel and stirred. In the reaction chamber, metal silicon and alkali contained in the grinding waste liquid react to generate silicate and generate hydrogen gas. On the other hand, agglomeration of abrasive grains not involved in this reaction is promoted in the reaction solution by the action of alkali.

JP 11-48146 A JP 2005-349507 A

In the above prior art, since the reaction solution is stirred, the agglomerated solid is difficult to settle. Moreover, the aggregated solid matter tends to rise by interfering with the hydrogen gas generated in the reaction chamber. For this reason, it is not easy to precipitate the agglomerate and continuously remove it from the reaction chamber, and so-called continuous processing is easy, in which grinding waste liquid and alkali are continuously supplied and reaction residue is continuously discharged. Not.
In addition, when the agglomerates rise and cover the liquid surface, the liquid surface becomes muddy, and hydrogen gas bubbles generated in the reaction chamber cause a foaming phenomenon on the muddy liquid surface, which bursts. In such a case, there is a problem that the liquid containing the solid matter is scattered. In particular, when the droplets adhere to the hydrogen gas exhaust passage, the exhaust passage may be blocked by solid matter contained in the splash.

  The technical problem of the present invention is to solve the above-mentioned problems, prevent interference between the gas generated by the reaction between the metal component and the alkali and the residual solid that settles after the reaction, and remove the solid after the reaction outside the system. It is an object of the present invention to provide a gas generating reaction apparatus having a solid-gas separation function, which can be continuously processed while being discharged efficiently, and which can form the entire apparatus compactly.

In order to solve the above-described problems, the present invention is described as follows, for example, based on FIGS. 1 to 3 showing an embodiment of the present invention.
That is, the present invention relates to a gas generation reaction apparatus having a solid-gas separation function, which is a reaction apparatus that generates a gas by reacting a raw material containing a metal component with an alkali in a liquid, and has a cylindrical shape arranged vertically. Reactor body (40) and a screw (41) arranged inside the reactor body (40), the reactor body (40), the raw material inlet (43) and gas outlet (54) at the top And the liquid outlet (60) is opened in the lower part, and the screw (41) includes a vertical shaft part (51) and a spiral blade (56) fixed around the shaft part (51), A spiral reaction chamber (57) extending in the vertical direction by the spiral blade (56) is formed in the reactor body (40), and the raw material inlet (43) and the reaction chamber (57) are formed in the reaction chamber (57). gas outlet (54) and a liquid outlet (60) and allowed to communicate with each said raw materials are fed through a raw material inlet of the, by moving the reaction chamber of the downward liquid outlet In the process, the gas reacts with the alkali to generate the gas, and the gas spirally rises along the lower surface of the spiral blade and is discharged from the gas outlet. The residual solids made of solids not involved in the reaction or produced by the reaction are guided down the spiral reaction chamber along the upper surface of the spiral blade and discharged from the liquid outlet. And

  The raw material containing the metal component is introduced from the raw material inlet, moves through the spiral reaction chamber to the lower liquid outlet, and reacts with alkali in the process to generate gas. The gas generated by this reaction rises spirally along the lower surface of the spiral blade and is discharged from the gas outlet. Among the above raw materials, the residual solids composed of solids not involved in the reaction or solids generated by the reaction are guided downward in the spiral reaction chamber along the upper surface of the spiral blade. When reaching the lower part, it is discharged from the liquid outlet together with a part of the reaction liquid.

You may use the raw material containing said metal component as a granular form. However, if this raw material is a so-called slurry in which solids such as powder are dispersed in a liquid, the raw material can be easily introduced without allowing air to flow into the reaction chamber. It is particularly preferred if it occurs. In this case, if a thickener is added to the above slurry, solids do not easily precipitate in the liquid, and the uniformly dispersed state is maintained. It is preferable because it can be easily and reliably sent by a pump or the like, and the metal component and the alkali can be reacted efficiently in the reaction chamber. As these thickeners, those which do not affect the reaction between the metal component and the alkali and the reaction products are preferable, and specific examples include carboxymethyl cellulose.
The alkali may be introduced from the raw material inlet in the form of an aqueous solution together with the raw material, or may be introduced from an inlet opened separately, and may be stored in the reaction chamber in advance. Is possible.

The metal component mentioned above is a component that reacts with an alkali to generate gas, and specifically includes metal silicon, metal aluminum, aluminum nitride, or the like, but is not limited to a specific component.
As the raw material containing this metal component, for example, waste liquid of grinding liquid in which abrasive grains are dispersed in a coolant used for cutting silicon wafers, or aluminum dross containing aluminum nitride can be used. The raw materials used in the above are not limited to these, and may be, for example, metal silicon or metal aluminum powder.

  In addition, the alkali can be used by appropriately selecting, for example, sodium hydroxide, sodium hydrogen carbonate, calcium hydroxide, potassium hydroxide, or a mixture thereof as necessary, and the concentration thereof is also particularly limited. Not. Further, as the alkali, waste alkali discharged from various other processes can be used.

The screw may be fixed to the reactor main body. In this case, the apparatus structure can be simplified, maintenance is easy, and it can be carried out at a low cost, which is preferable.
However, the above-mentioned screw may be supported so as to be rotatable around the axis in the reactor main body. In this case, the raw material containing the metal component can be guided downward at a desired speed by the rotation of the screw. The reaction time with the alkali in the reaction chamber can be controlled, which is preferable.

  The reaction between the metal component and the alkali is started by heating to a predetermined temperature and proceeds rapidly. However, when the reaction proceeds, heat is generated and the temperature of the reaction solution rises. For this reason, in order to control the reaction rate, at least one of the site along the peripheral wall of the reactor main body and the inside of the shaft portion is provided with a temperature adjusting means for controlling the temperature in the reaction chamber. Placement is preferred. As the temperature adjusting means, specifically, a heating means may be arranged on the peripheral wall or the shaft portion, and the temperature adjusting means may be configured to control the heating device. Alternatively, the temperature adjusting means may be arranged on the peripheral wall. A medium circulating means for circulating a heat medium or a refrigerant controlled at a predetermined temperature into the jacket formed along the shaft or the shaft portion may be used, and these may be used alone or in combination.

  If the liquid level in the reaction chamber rises excessively, the gas outlet may be blocked. Therefore, the amount of raw material charged into the reaction chamber and the amount of residue discharged from the reaction chamber may be adjusted to adjust the liquid level. It is necessary to control the surface to a predetermined range position. In order to detect the liquid level position, a liquid level gauge may be provided in the reactor main body, but a liquid level control tank is disposed on the side of the reactor main body, and the liquid level control tank If the lower part is connected to the liquid outlet via the communication path and the liquid level in the liquid level control layer is detected, the number of members arranged in the reaction chamber is reduced and the structure of the reactor body is simplified. This is preferable.

  Since the drainage path connected to the above liquid outlet is likely to have residual solids attached thereto, if a washing water tank is connected to the drainage path via the washing water supply path, the attached residual solids can be easily removed. This is preferable because it can be washed away and, for example, the opening / closing operation of the drain valve attached to the drain passage can be maintained satisfactorily.

  When hydrogen gas is generated by the reaction between the metal component and the alkali, it is necessary to consider that hydrogen and air are not mixed in the reactor main body or piping. Therefore, if a pressurized gas supply path is connected to the upper part of the reactor main body via a gas supply valve, a pressurized gas such as nitrogen gas is supplied to the reactor main body prior to the hydrogen gas generation reaction. It is preferable that the air remaining in the reactor main body and the piping can be replaced by supplying the gas into the reactor. Furthermore, in this case, there is also an advantage that the residue in the reaction chamber can be quickly discharged from the liquid outlet by introducing the pressurized gas into the reactor main body after the reaction is completed.

  The gas discharged from the gas outlet may contain mist of the reaction solution generated in the reaction chamber. In addition, an abnormally large amount of foaming may occur in the reaction chamber, and this foam may overflow from the gas outlet. For this reason, if an anti-foaming device capable of spraying water is placed in the upper space inside the reactor body, the above abnormal foaming state can be easily eliminated, and the overflow of bubbles from the gas outlet is prevented. This is preferable.

  Since the present invention is configured and operates as described above, the following effects can be obtained.

(1) Residual solids such as non-reacted solids and reaction products settle spirally along the upper surface of the spiral blade, while the gas generated by the reaction rises along the lower surface of the spiral blade. To go. For this reason, it is possible to prevent the rising gas and the solid matter that settles from interfering with each other, prevent the solid matter from rising due to the generated gas, and satisfactorily settle the aggregated solid matter. As a result, the residual solid can be continuously taken out from the liquid outlet during the reaction, and the raw material containing the metal component can be continuously processed.

(2) Moreover, since the liquid surface can be prevented from being covered with a solid material, the liquid surface generated by the aggregation of the solid material can be prevented from foaming and the foamed liquid surface from rupturing, and the reaction liquid can be prevented from scattering. Thus, it is possible to reduce the possibility that the gas outlet is blocked due to the adhesion of the droplets.

(3) Since the raw material introduced from the raw material inlet is guided from the upper side to the lower side in the spiral reaction chamber along the spiral blade, the path is longer than the case where the raw material is guided linearly from the inlet to the outlet. Will be moved. As a result, even if the length of the reactor main body is shortened, a sufficient reaction time between the raw material and the alkali can be ensured and the reaction can be efficiently performed, and the entire apparatus can be formed compactly.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.
1 and 2 show a first embodiment of the present invention, FIG. 1 is a flow diagram showing a schematic configuration of a waste liquid treatment apparatus, and FIG. 2 is a longitudinal sectional view of a gas generation reaction apparatus having a solid-gas separation function. is there.

  A waste liquid treatment apparatus (1) shown in FIG. 1 is used to regenerate a waste liquid of a grinding liquid used for cutting a silicon wafer or the like in which abrasive grains are dispersed in a coolant. The waste liquid treatment apparatus (1) includes a gas generation reaction apparatus (2) having a solid-gas separation function, and a raw material supply section (3) and an alkali supply section (4) are respectively provided with a raw material supply path (5). And an alkali supply path (6) connected to the upper part of the gas generating reaction apparatus (2). The raw material supply unit (3) includes a raw material tank (3a) and a water tank (3b), and slurry-like grinding waste liquid is stored in the raw material tank (3a). The alkali supply unit (4) includes an alkali tank (4a) and a water tank (4b), and an alkali solution having a predetermined concentration, for example, an aqueous solution of sodium hydroxide, is accommodated in the alkali tank (4a). A supply pump (7) and a supply valve (8) are attached to the raw material supply path (5) and the alkali supply path (6), respectively.

  The raw material supply path (5) is connected to a pressurized gas supply path (10) via a gas supply valve (9), and a nitrogen gas tank ( From 11), nitrogen gas can be supplied into the gas generating reactor (2).

  The upper end of the gas generation reaction device (2) is connected to the hydrogen gas storage tank (13) via the gas discharge path (12). The gas discharge path (12) includes a mist recovery trap (15), a gas cooler (16), a drain trap (17), between the gas generation reactor (2) and the hydrogen gas storage tank (13). A flow meter (18) is arranged in order. In the upper space in the gas generating reaction device (2), the spray detector (21) of the foam detector (19) and the defoaming device (20) is arranged. The spray device (21) is a water tank (22 ).

  A heating device (23) controlled by a temperature adjusting means (25) is provided around the gas generating reaction device (2). The heating device (23) is controlled by the temperature adjusting means (25) based on the output of the temperature sensor (26) for detecting the temperature in the gas generating reaction device (2). The inside is heated to a predetermined temperature.

The lower part of the gas generation reactor (2) having the above-mentioned solid-gas separation function is connected to the liquid recovery tank (28) via the drainage path (27), and the middle part of the drainage path (27) Further, a drain cooler (29), a buffer tank (30), and a drain valve (31) are provided in this order. The refrigerant supplied from the chiller unit (32) is circulated through the drain cooler (29) and the gas cooler (16).
In addition, a washing water tank (34) is connected to the drainage passage (27) on the upstream side of the drainage valve (31) via a washing water supply passage (33). A washing water supply pump (35) and a washing water supply valve (36) are arranged in the supply path (33).

  A liquid level control tank (37) is disposed on the side of the gas generation reaction apparatus (2), and the lower part of the liquid level control tank (37) is a gas generation reaction apparatus having a solid-gas separation function ( Directly below 2), it communicates with the drainage channel (27) via the communication channel (38). A level sensor (39) is attached to the liquid level control tank (37), and the liquid level in the gas generation reactor (2) is detected through the liquid level in the liquid level control tank (37). Is done.

Next, a specific structure of the gas generation reaction apparatus (2) having the above-mentioned solid-gas separation function will be described based on FIG. 2 with reference to FIG.
As shown in FIG. 2, the gas generating reactor (2) includes a cylindrical reactor main body (40) arranged in a substantially vertical direction, and a screw (41) arranged inside the reactor main body (40). With.
The reactor body (40) has a raw material inlet (43), a temperature sensor mounting hole (44), and a pressure detection port (45) at the top of the peripheral wall (42), and this raw material inlet (43) The raw material supply path (5) is connected to the alkali supply path (6) and the pressurized gas supply path (10) via the downstream portion of the raw material supply path (5). The temperature sensor (26) is mounted in the temperature sensor mounting hole (44), and the pressure detection device (47) and the safety device (46) are connected to the gas escape path (46) connected to the pressure detection port (45). 48) is attached.

  A flange (50) is fixed to the outer surface of the upper end of the reactor main body (40), and a mounting flange (52) fixed to the shaft portion (51) of the screw (41) is a flange (50). ) Is fixed via a gasket (53). A gas outlet (54) is opened on the mounting flange (52) so as to face the reactor body (40), and the gas outlet (12) is connected to the gas outlet (54). It is.

  The shaft portion (51) is disposed along the vertical axis (55) in the reactor main body (40), and a spiral blade (56) is fixed around the shaft portion (51). The spiral blade (56) forms a spiral reaction chamber (57) extending vertically in the reactor main body (40). The raw material inlet (43) and the gas outlet (54) communicate with the reaction chamber (57).

  The heating device (23) is formed outside the peripheral wall (42) of the reactor main body (40), and the heating device (23) is controlled by the temperature adjusting means (25). . A circulation path (58) extending in the vertical direction is formed in the shaft portion (51), and the cooling water (59) is circulated through the circulation path (58). The circulation path (58) constitutes a second temperature adjusting means (25) for controlling the temperature in the reaction chamber (57).

  A liquid outlet (60) communicating with the reaction chamber (57) is opened at a lower portion of the reactor main body (40), and the drainage passage (27) is formed in the liquid outlet (60). Connected.

Next, a procedure for treating grinding waste liquid using the above-described waste liquid treatment apparatus will be described.
First, after exhausting the air in the reactor main body (40) and the piping by an exhaust device (14) such as a vacuum pump, the pressurized gas supply path (10) into the reactor main body (40). Nitrogen gas (61) is supplied to remove air remaining in the reactor main body (40) and the pipe connected thereto.
Next, a predetermined amount of the alkaline solution (63) is injected from the alkali tank (4a) into the reaction chamber (57) of the reactor body (40) and heated to a predetermined temperature, for example, 80 ° C. Subsequently, the slurry-like grinding waste liquid (62) is supplied from the raw material tank (3a) into the reaction chamber (57), and the alkali solution (63) is supplied from the alkali tank (4a).

  In the reaction chamber (57), the reaction liquid in which the grinding waste liquid and the alkaline solution are mixed is heated to a predetermined temperature such as 80 ° C. by the heating device (23). As a result, the metal silicon contained in the grinding waste liquid reacts with the alkali and dissolves to produce silicate and generate hydrogen gas (64). The hydrogen gas (64) spirally rises in the reaction chamber (57) along the lower surface of the spiral blade (56), and is discharged from the gas outlet (54) to the gas discharge path (12). On the other hand, solids (65) that are not involved in the reaction, such as abrasive grains contained in the grinding waste liquid, agglomerate due to the action of the alkaline solution, along the upper surface of the spiral blade (56), the reaction chamber (57) When it reaches the lower part of the reaction chamber (57), it is discharged as a residual solid together with a part of the reaction liquid from the liquid outlet (60) to the drainage path (27).

When the temperature of the reaction solution rises due to the above reaction, the cooling water (59) is circulated through the circulation path (58) in the shaft (51), and the inside of the reaction chamber (57) is controlled to a predetermined temperature.
The liquid level of the reaction liquid in the reaction chamber (57) is detected by a level sensor (39) attached to the liquid level control tank (37), and the raw material supply part (3) and alkali supply part (4). By adjusting the supply amount from the drainage and the drainage amount from the drainage channel (27), the vertical position within the predetermined range is controlled.

  The hydrogen gas (64) generated by the reaction may foam as a result of mutual interference with the residual solid. When the foamed hydrogen gas is detected by the foam detector (19), water is sprayed from the sprayer (21) of the defoamer (20) installed in the upper space of the reaction chamber (57). Is defoamed.

  The hydrogen gas discharged from the gas outlet (54) to the gas discharge passage (12) is then guided to the mist recovery trap (15) to remove mist-like water containing alkali components. The hydrogen gas from which the mist has been removed is cooled by a gas cooler (16) and condensed water vapor is condensed.After the condensed water is removed by a drain trap (17), the pressure is adjusted to a constant pressure by a pressure regulating valve. While being adjusted, the hydrogen gas is stored and guided to the hydrogen gas storage tank (13). At this time, the hydrogen gas generation amount is measured by the flow meter (18) provided in the gas discharge path (12), and the raw material supply amount and the alkali supply amount are adjusted based on the measured value, and the reaction chamber (57 ) Is controlled so as to stabilize the amount of hydrogen gas generated.

  On the other hand, the residual solid matter and the reaction liquid discharged from the liquid outlet (60) to the drainage passage (27) are cooled by the drainage cooler (29), and the hydrogen gas remaining in the buffer tank (30) is reduced. After being separated, it is stored in the liquid recovery tank (28). The residual solid recovered in the liquid recovery tank (28) is separated from the reaction liquid by filtration, centrifugation, etc. in the subsequent processing step, but the metal silicon contained in the grinding waste liquid is Since it is consumed in the reaction, almost no metallic silicon remains in the residual solid or reaction solution. Accordingly, the abrasive grains are regenerated well from the residual solids, and the coolant is regenerated well from the reaction liquid.

  Since the reaction liquid flowing through the drainage path (27) contains residual solids, the residual solids may adhere to the drainage valve (31) that opens and closes the drainage path (27). . Therefore, when the drain valve (31) is opened and closed, the cleaning water is supplied from the cleaning water tank (34) through the cleaning water supply passage (33), whereby the residual solids are discharged from the drain valve. The liquid is smoothly guided to the liquid recovery tank (28) without adhering to the inside of (31). The drain valve (31) is preferably formed of a material having excellent wear resistance such as ceramic so as not to be worn early by abrasive grains contained in the residual solid.

  In the first embodiment, the waste liquid treatment apparatus (1) including one gas generation reaction apparatus (2) has been described. In this case, if the raw material supply amount is increased in order to increase the processing amount per hour, the residence time in the reaction chamber is shortened, the reaction efficiency is lowered, and the unreacted substances discharged from the gas generating reactor are increased. For this reason, in order to increase the throughput while maintaining high reaction efficiency, it is necessary to make the reactor body longer or to increase its size. However, in the present invention, by providing a plurality of gas generating reactors, it is possible to increase the throughput while maintaining high reaction efficiency.

  The plurality of gas generating reactors may be arranged in parallel, and the raw material supply unit may be connected to each gas generating reactor, or each gas generating reactor is arranged in series, You may connect a raw material supply part only to the gas generating reaction apparatus of the most upstream side. In particular, when the gas generating reactors are arranged in series, the structure of the raw material supply section such as the raw material supply path can be simplified, and the downstream gas can be determined based on the reactivity in the upstream gas generating reactor. By adjusting the reaction in the generation reaction apparatus, the overall reaction efficiency can be controlled, for example, by suppressing unreacted residues to a low level, which is preferable. Furthermore, in this invention, it is also possible to arrange | position several gas generation reaction apparatuses combining the parallel form and the serial form.

  FIG. 3 is a schematic configuration diagram of a waste liquid treatment apparatus showing a second embodiment of the present invention. In the second embodiment, the waste gas treatment device (1) is provided with four gas generation reaction devices (2), and the gas generation reaction devices (2) are arranged in series with each other. That is, the raw material supply (3) and the alkali supply section (4) are connected to the upper part of the most upstream gas generation reaction apparatus (2), and the upper part of the downstream gas generation reaction apparatus (2) is Each is connected to the lower part of the upstream gas generation reactor (2) via a liquid feed path (24). The lowermost part of the gas generation reactor (2) on the most downstream side is connected to the liquid recovery tank (28) via the drainage passage (27).

  A reaction chamber (57) is formed in each gas generating reaction device (2), and a gas storage space (66) is provided above each reaction chamber (57). Each of the reaction chambers (57) and the gas storage space (66) communicate with each other via a liquid return path (67). A gas storage space (66) of each gas generation reaction device (2) is connected to a hydrogen gas storage tank (13) via a gas discharge path (12).

  The liquid feeding path (24) is connected to a slightly lower position in the upper part of the gas generating reaction apparatus (2) as it goes downstream. This is because, in particular, when the viscosity of the slurry-like raw material is increased by adding the above-mentioned thickener, when the pipe resistance due to the above-described liquid feeding path (24) is large, the gas generating reaction apparatus (2) becomes more downstream. There is a tendency that the liquid level in the inside tends to be low, and it is adapted to this. However, in the present invention, if there is no possibility that the reaction solution overflows from the reaction chamber (57) to the gas storage space (66) in the upstream gas generation reactor (2) due to the pipe resistance, You may connect each liquid sending path (24) to the substantially same height position of each gas generation reaction apparatus (2).

An individual drainage channel (49) is connected to the lower part of the gas generation reactor (2). The individual drainage channel (49) is closed during normal reaction processing, and is opened during maintenance when an abnormality occurs or during cleaning after completion of the reaction.
In the second embodiment, the alkali supply section (4) is connected to the upper part of the most upstream gas generation reaction apparatus (2). However, in the present invention, each gas generation reaction apparatus ( You may connect an alkali supply part (4) to the upper part of 2), respectively.
In the second embodiment, the case where the four gas generating reactors (2) are provided has been described. However, in the present invention, the number of gas generating reactors is not limited to a specific number, and the number is three or less. Or five or more.

Next, a processing procedure for grinding waste liquid using the above-described waste liquid treatment apparatus will be described.
In the waste liquid treatment apparatus (1) provided with the plurality of gas generation reaction apparatuses (2), the slurry-like raw material (62) supplied from the raw material supply section (3) is fed upstream by the supply pump (7). To the side gas generating reactor (2). The slurry-like raw material passes through the reaction chamber (57) of the gas generating reactor (2), and then upstream to the remaining gas generating reactors (2) via the liquid feeding path (24). Is sent to the downstream side in order and passes through the inside. At this time, since each gas generating reactor (2) is configured to be tightly sealed with respect to the external space, the lower part of the upstream gas generating reactor (2) is the upper part of the downstream gas generating reactor (2). The slurry-like raw material is reliably sent to the downstream gas generating reaction device (2) with a simple configuration that is simply connected to the gas supply passage (24).

  The metal component contained in the raw material reacts with the alkali (63) supplied from the alkali supply unit (3) while passing through the reaction chamber (57) of each gas generating reactor (2). As a result, hydrogen gas is generated in each reaction chamber (57). The hydrogen gas (64) is guided and stored in the hydrogen gas storage tank (13) from the gas storage space (66) of each gas generation reaction device (2) through the gas discharge path (12). At this time, in each gas generating reactor (2), the reaction liquid may overflow from the reaction chamber (57) into the gas storage space (66) due to foaming of hydrogen gas or the like. In this case, after the foaming is eliminated, the overflowing reaction liquid is returned to the reaction chamber (57) through the liquid return path (67).

  Since the metal component contained in the slurry-like raw material sequentially passes through all the gas generation reactors (2), it comes into contact with the alkali for a long time. As a result, even if the supply amount from the raw material supply unit (3) is increased to increase the processing amount, it reacts efficiently and sufficiently until there is almost no unreacted material. The sufficiently reacted liquid is discharged together with the remaining solids (65) from the lowermost part of the gas generation reactor (2) on the most downstream side, and is guided to the liquid recovery tank (28) through the drainage path (27). Is housed. Other configurations are the same as those in the first embodiment, and the description thereof will be omitted because it operates in the same manner.

  In each of the above embodiments, the case where the grinding waste liquid is processed has been described. However, the gas generation reaction apparatus having the solid-gas separation function of the present invention and the processing apparatus equipped with the same are not only used for regeneration of the coolant, but also for example, a hydrogen gas generation apparatus using aluminum particles as a raw material, and detoxification of various waste liquids. It can also be used as a processing device. In these cases, the residual solid recovered in the liquid recovery tank does not have a metal component that reacts with alkali to generate gas, or has been greatly reduced. After making adjustments, it can be safely disposed of.

  For example, aluminum nitride contained in aluminum dross has a problem that ammonia gas may be generated when it reacts in contact with rainwater and cannot be discarded as it is in a landfill. Therefore, in order to solve this problem, the aluminum dross can be used as a raw material, and the above-described treatment apparatus can be used as an aluminum dross detoxification treatment apparatus.

  In this case, aluminum dross and an alkaline solution are charged into the reaction chamber, whereby aluminum nitride and alkali react with each other in the reaction chamber to generate aluminum hydroxide and generate ammonia gas. After the ammonia gas is discharged from the gas outlet, it is recovered in a form such as liquefied ammonia or concentrated aqueous ammonia by a method such as condensation. On the other hand, the aluminum hydroxide is reacted as a residual solid from the liquid outlet. It is discharged together with a part of the liquid recovery tank.

In said 1st Embodiment, said screw was fixed to the reactor main body so that rotation was impossible. However, in the present invention, this screw may be supported so as to be rotatable around the axis in the reactor main body. In this case, if the screw is rotated at a high speed, the reaction solution is stirred and the settling of the residual solid matter is hindered. Therefore, the screw is preferably rotated at a low speed so that the precipitate is not excessively wound.
When the screw is rotated in this manner, the moving speed of the solid substance, that is, the residence time in the reaction chamber can be adjusted, and the metal component can be controlled so that it sufficiently reacts with the alkali in the reaction chamber. The reaction efficiency can be further increased by reducing the discharge of the reactants.

  The gas generation reaction apparatus having a solid-gas separation function described in each of the above embodiments is exemplified to embody the technical idea of the present invention, and the structure and arrangement of each member are shown in this embodiment. The present invention is not limited to this, and various modifications can be made within the scope of the claims of the present invention.

For example, in the first embodiment, a heating device is arranged outside the peripheral wall of the reactor main body, and the cooling water is circulated through a circulation path provided in the shaft portion of the screw. However, in the present invention, instead of this, a jacket may be formed outside the peripheral wall of the reactor main body, the cooling water may be circulated through the jacket, and the heat medium may be circulated within the shaft portion. It is also possible to configure the heating medium and the refrigerant to be switched and supplied to either one of the jacket and the circulation path in the shaft portion, and to omit the other.
In each of the above embodiments, since the slurry-like raw material is used, the raw material can be easily supplied into the reaction chamber without mixing air, but in the present invention, for example, the granular raw material is added using a water sealing mechanism or the like. You may comprise so that it may supply in a reactor main body.
Needless to say, the types and concentrations of the metal components and alkalis contained in these raw materials are not limited to the above embodiments and specific numerical ranges.

  The gas generating reaction apparatus having a solid-gas separation function of the present invention prevents the interference between the gas generated by the reaction between the metal component and the alkali and the residual solids settled after the reaction, thereby improving the reaction efficiency between the raw material and the alkali. It can be processed continuously while maintaining a high level, and the entire device can be made compact, so that waste generated from the semiconductor manufacturing field, etc. is generated along with recycling and detoxification. It is also suitably used for a recovery device for hydrogen gas or the like.

It is a flowchart which shows schematic structure of the waste-liquid processing apparatus of 1st Embodiment of this invention. It is a longitudinal cross-sectional view of the gas generation reaction apparatus which has a solid-gas separation function of 1st Embodiment of this invention. It is a schematic block diagram of the waste liquid processing apparatus of 2nd Embodiment of this invention.

1 ... Treatment device (waste liquid treatment device)
2 ... Gas generating reactor with solid-gas separation function
10 ... Pressurized gas supply path
11… Nitrogen gas tank (gas supply tank)
20 ... Defoaming device
25 ... Temperature adjustment means
27… Drainage path
33… Washing water supply channel
34… Washing water tank
37 ... Liquid level control tank
40 ... Reactor body
41 ... Screw
42 ... Surrounding wall
43 ... Raw material inlet
54… Gas outlet
55 ... axis
56 ... Spiral feather
57 ... Reaction chamber
60 ... Liquid outlet

Claims (10)

A reaction apparatus for generating a gas by reacting a raw material containing a metal component with an alkali in a liquid,
A cylindrical reactor body (40) arranged in the vertical direction and a screw (41) arranged inside the reactor body (40),
The reactor body (40) has a raw material inlet (43) and a gas outlet (54) opened at the top and a liquid outlet (60) opened at the bottom,
The screw (41) includes a vertical shaft portion (51) and a spiral blade (56) fixed around the shaft portion (51), and a spiral reaction chamber (57) extending in the vertical direction by the spiral blade (56). Is formed in the reactor body (40).
The raw material inlet (43), the gas outlet (54) and the liquid outlet (60) are communicated with the reaction chamber (57), respectively .
The raw material is introduced from the raw material inlet, and the reaction chamber is moved to the lower liquid outlet side. In the process, the raw material reacts with the alkali to generate the gas. The upper surface of the spiral blade is a solid residue that is spirally raised along the lower surface of the spiral blade and is discharged from the gas outlet and is made up of the solid material that is not involved in the reaction and the solid material generated by the reaction. A gas generation reaction apparatus having a solid-gas separation function, wherein the gas is guided downward in the spiral reaction chamber and discharged from the liquid outlet .   The gas generating reaction device having a solid-gas separation function according to claim 1, wherein the screw (41) is fixed in the reactor main body (40).   The gas generating reaction apparatus having a solid-gas separation function according to claim 1, wherein the screw (41) is rotatably supported around an axis (55) in the reactor main body (40).   Temperature control for controlling the temperature in the reaction chamber (57) on at least one of the site along the peripheral wall (42) of the reactor body (40) and the inside of the shaft portion (51) The gas generating reaction apparatus having a solid-gas separation function according to any one of claims 1 to 3, wherein means (25) is arranged.   The liquid level control tank (37) is disposed on the side of the reactor main body (40), and the lower part of the liquid level control tank (37) communicates with the liquid outlet (60). 5. A gas generating reaction apparatus having a solid-gas separation function according to any one of 4 above.   The washing water tank (34) is connected to the drainage passage (27) connected to the liquid outlet (60) via the washing water supply passage (33), according to any one of claims 1 to 5. A gas generation reaction apparatus having the solid-gas separation function.   The solid-gas separation according to any one of claims 1 to 6, wherein a gas supply tank (11) is connected to an upper portion of the reactor main body (40) via a pressurized gas supply path (10). A gas generating reactor having a function.   The gas generation reaction having a solid-gas separation function according to any one of claims 1 to 7, wherein a defoaming device (20) capable of spraying water is disposed in an upper space in the reactor main body (40). apparatus.   The gas having a solid-gas separation function according to any one of claims 1 to 8, wherein the raw material is a waste liquid of a grinding liquid in which abrasive grains are dispersed in a coolant used for cutting a silicon wafer or the like. Generation reactor.   The gas generation reaction apparatus having a solid-gas separation function according to any one of claims 1 to 8, wherein the raw material is aluminum dross containing aluminum nitride.

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