JP2008007336A - Ozone concentrating apparatus and method for driving ozone concentrating apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To suppress the generation of ozone decomposition in a liquid sealing section, to eliminate the risk of the breakage of the apparatus, and to realize stable liquid ozone production. <P>SOLUTION: A filler 8 is filled into liquid seal piping 6, and the inlet side and outlet side are provided with gauges 31, 32. By the control of a pressure regulation means V1 or the like practiced based on information regarding a liquid level detected by the gauges 31, 32, the feed of liquid ozone to the liquid seal piping 6 and the fixed holding of the liquid level in a separation boundary face 7 are made possible, the abnormal storage on the side of the separation boundary face 7 and the discharge of the liquid ozone to a vaporization section 2 are prevented, also, the liquid ozone is satisfactorily introduced into the vaporization section 2 with the filler 8 by its capillary force, and, on the other hand, the heat capacity in heat absorption is increased, and further, the liquid ozone in the liquid seal piping 6 is reduced. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to an ozone concentrator for concentrating ozone gas generated by an ozonizer and a method for operating the ozone concentrator.

For example, high-concentration ozone gas used for manufacturing semiconductors and the like is generated by concentrating ozone gas containing ozone with an ozone concentrator. As this ozone concentrator, ozone gas generated by an ozone generator (ozonizer) based on air or oxygen is cooled in a tank-like ozone liquefaction chamber and separated into liquid ozone and oxygen at the boundary of the boundary, Oxygen is exhausted from the top of the ozone liquefaction chamber, liquid ozone is stored at the bottom of the ozone liquefaction chamber, and the liquid ozone stored in the liquefaction chamber passes through a communication pipe (liquid seal) that is liquid-sealed with the liquid ozone. There is known a device that introduces into a tank-shaped ozone vaporization chamber (vaporization section) and heats liquid ozone in the ozone vaporization chamber to vaporize it to obtain concentrated ozone (high concentration ozone gas) (for example, see Patent Document 1). ).
JP-A-1-257103

Here, high-concentration ozone gas (generally, the volume ratio of ozone is 10% or more) is, for example, when there are triggers such as catalytic action of metal fine particles, high temperature, impact force, and organic gas decomposed by ozone. Decomposes and generates heat (O ₃ → 1.5O ₂ +143 kJ / mol), and other ozone gas is heated and self-decomposed by the heat generated during the decomposition, or liquid ozone is heated and vaporized to self-decompose. There is a risk of causing.

  Therefore, in the concentrating device, if ozone decomposition occurs in the liquid seal part due to the trigger or the like, this ozone decomposition is chained, and the temperature rapidly rises and liquid ozone is vaporized and decomposed. Since the volume expansion becomes as large as about 1000 times, the pressure increases rapidly, which may cause damage to the apparatus.

  The present invention has been made to solve such a problem, and an ozone concentrating device and an ozone concentrating device capable of suppressing the occurrence of ozonolysis applied to a liquid seal portion and eliminating the possibility of damage to the device. It aims at providing the operating method of an apparatus.

  Here, as a result of intensive studies, the present inventors have found that in the ozone concentrator having the above-described configuration, if the liquid ozone is present at the bottom and the liquid seal portion of the liquefaction chamber and the amount of liquid ozone is large, When decomposition occurs, a large amount of liquid ozone is vaporized and chained ozone decomposition occurs, and it is difficult to suppress damage to the device due to rapid expansion of the volume. It has been found that if the amount of ozone vaporization is reduced as much as possible, the influence of chain ozone decomposition due to the vaporization of liquid ozone can be suppressed.

  The inventors of the present invention have found that such an ozone concentrating device is effective in that the liquid sealing portion is filled with a filler that develops capillary force and the liquid ozone is gradually supplied to the vaporizing portion. In such an ozone concentrator, while the liquid ozone is well guided to the vaporizing part by the capillary force of the filler in the liquid sealing part and is vaporized, the generated heat is generated in the liquid sealing part even if ozone decomposition occurs. In this case, the amount of liquid ozone is absorbed by the heat capacity of the filler and the amount of liquid ozone is reduced by the filler, thereby suppressing chain ozone decomposition due to vaporization of liquid ozone and eliminating the possibility of destruction of the apparatus. Can do.

  Here, in such an ozone concentrator, in the case of starting up or resuming operation after being stopped for a long time, the liquid seal portion is filled with air, and a good capillary tube with a filler is used. Force cannot be expressed, liquid ozone is stored more than specified at the inlet side of the liquid seal (abnormal storage), and in the unlikely event that abnormal decomposition of ozone occurs, there is a risk of damage increasing, so it is good It was found that liquid ozone needs to be filled from the specified position on the inlet side of the liquid seal portion to the outlet side in order to develop capillary force. Also, when the pressure on the inlet side of the liquid seal part is suddenly increased when filling with liquid ozone, there is a risk that liquid ozone may be ejected on the vaporization part side, while on the other hand, if the pressure on the vaporization part side is increased, It has also been found that when abnormal storage of excessive liquid ozone occurs on the separation boundary surface side, extremely large damage is caused when abnormal decomposition of ozone occurs.

  Therefore, the ozone concentrator according to the present invention is a cooling means for cooling the ozone gas generated by the ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensable gas, and heating the liquid ozone separated by the cooling means. A vaporization part that vaporizes and obtains concentrated ozone, a liquid sealing part that seals between the vaporization part and the separation boundary surface between liquid ozone and non-condensable gas, and a filler that fills the liquid sealing part and develops capillary force And a first information acquisition means for acquiring information on the liquid level on the separation boundary surface, and a second information acquisition means for acquiring information on the liquid level on the vaporization part side of the liquid sealing part. And

  According to such an ozone concentrator, since the first information acquisition means acquires information on the liquid level on the separation boundary surface (the height of the liquid level, the presence or absence of liquid at the specified position, etc.), It is possible to monitor whether there is a sudden fluctuation in the liquid level on the separation boundary surface side of the liquid sealing part due to excessive application of pressure to the separation boundary surface of the liquid sealing part when filling with liquid ozone, etc. In addition, it is possible to monitor whether or not the liquid level of liquid ozone on the separation boundary surface side of the liquid sealing portion is kept constant. In addition, since the second information acquisition means acquires information on the liquid level on the vaporization unit side, it is possible to monitor whether or not the liquid ozone on the separation boundary surface side flows well into the liquid seal part on the vaporization unit side, It is possible to monitor whether or not the liquid level of the liquid ozone on the vaporizing part side is suddenly changed and whether or not the liquid level on the vaporizing part side is kept constant when the liquid ozone is filled in the liquid sealing part. . By adjusting the pressure on the separation boundary side based on the monitor information acquired in this way, abnormal storage on the separation boundary side and ejection of liquid ozone at the vaporization section are prevented, thereby stabilizing It is possible to produce liquid ozone, and even if abnormal decomposition of liquid ozone occurs, the influence can be reduced. In addition, the liquid ozone is well guided to the vaporization part due to the capillary force of the filler in the liquid seal part and vaporizes. On the other hand, even if ozone decomposition occurs, the generated heat is in the heat capacity of the filler in the liquid seal part. And the amount of liquid ozone is reduced by the filler, and chain ozone decomposition due to vaporization of liquid ozone is suppressed. Therefore, it is possible to generate stable liquid ozone and eliminate the possibility of damage to the apparatus.

  Here, examples of the information acquisition means include a capacitance level meter that measures a capacitance that changes depending on the liquid level, a differential pressure level meter that measures a pressure proportional to the liquid level, and the like.

  The ozone concentrator according to the present invention also comprises a cooling means for cooling the ozone gas generated by the ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensed gas, and heating the liquid ozone separated by the cooling means. A vaporization part that vaporizes and obtains concentrated ozone, a liquid sealing part that seals between the vaporization part and the separation boundary surface between liquid ozone and non-condensable gas, and a filler that fills the liquid sealing part and develops capillary force And a pressure adjusting means for adjusting the pressure on the separation boundary surface.

  According to such an ozone concentrator, the pressure on the separation boundary surface is adjusted by the pressure adjusting means. For example, by increasing the pressure on the separation boundary surface, it is possible to send liquid ozone into the liquid seal portion. Furthermore, it is possible to keep the liquid level at the separation boundary surface constant and prevent liquid ozone from being stored more than a specified amount on the inlet side (abnormal storage). Further, by reducing the pressure applied to the separation boundary surface by the pressure adjusting means, it is possible to prevent the discharge of liquid ozone in the vaporization section due to excessive application of pressure to the separation boundary surface. As described above, abnormal storage on the separation boundary side and ejection of liquid ozone at the vaporization section are prevented, thereby making it possible to generate stable liquid ozone, and by any chance, abnormal decomposition of liquid ozone occurs. However, the influence can be reduced. In addition, the liquid ozone is well guided to the vaporization part due to the capillary force of the filler in the liquid seal part and vaporizes. On the other hand, even if ozone decomposition occurs, the generated heat is in the heat capacity of the filler in the liquid seal part. And the amount of liquid ozone is reduced by the filler, and chain ozone decomposition due to vaporization of liquid ozone is suppressed. Therefore, it is possible to generate stable liquid ozone and eliminate the possibility of damage to the apparatus.

  Here, a gas pipe for deriving non-condensable gas is provided, and the liquid sealing part and the gas pipe are branched and connected to the outlet of the ozone flow path cooled by the cooling part of the cooling means, respectively, and the pressure adjusting means Is provided with respect to the gas piping, and it is preferable that a pressure adjusting chamber is connected upstream of the pressure adjusting means of the gas piping. When such a configuration is adopted, the liquid sealing portion and the gas pipe are branched and connected to the outlet of the ozone flow path, and the non-condensable gas is led out by the gas pipe. And since the quantity of the non-condensing gas to derive is adjusted by the pressure adjustment means provided in gas piping, the pressure with respect to a separation boundary surface is adjusted easily. At this time, since the pressure chamber connected to the gas pipe secures a certain amount of capacity, even if the volume of the gas pipe is small, rapid pressure fluctuation during adjustment by the pressure adjusting means is prevented. .

  The operation method of the ozone concentrator according to the present invention includes a cooling means for cooling ozone gas generated by an ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensed gas, and liquid ozone separated by the cooling means. A method for operating an ozone concentrator comprising: a vaporizing unit that heats and vaporizes to obtain concentrated ozone; and a liquid sealing unit that seals between a separation boundary surface between liquid ozone and non-condensable gas and the vaporizing unit. The liquid seal portion is filled with a filler that develops capillary force, and liquid ozone is added to the liquid seal portion while adjusting the pressure on the separation boundary surface side of the liquid seal portion and the pressure on the vaporization portion side of the liquid seal portion. It is characterized by charging.

  According to such an operation method of the ozone concentrator, the liquid sealing portion is filled with liquid ozone while gradually reducing the difference between the pressure on the separation boundary surface side and the pressure on the vaporization portion side. In this way, liquid ozone is prevented from being discharged and ejected at the vaporizing section, and stable generation of liquid ozone becomes possible. Even if abnormal decomposition of liquid ozone occurs, the influence can be reduced. In addition, the liquid ozone is well guided to the vaporization part due to the capillary force of the filler in the liquid seal part and vaporizes. On the other hand, even if ozone decomposition occurs, the generated heat is in the heat capacity of the filler in the liquid seal part. And the amount of liquid ozone is reduced by the filler, and chain ozone decomposition due to vaporization of liquid ozone is suppressed. Therefore, it is possible to generate stable liquid ozone and eliminate the possibility of damage to the apparatus.

  As described above, according to the present invention, by adjusting the liquid level with respect to the liquid sealing portion, it is possible to prevent abnormal storage on the separation boundary surface side and ejection of liquid ozone at the vaporization portion, so that stable generation of liquid ozone can be achieved. It becomes possible. As a result, even if abnormal decomposition of liquid ozone occurs, the damage can be reduced. In addition, the capillary force of the filler can lead the liquid ozone to the vaporization part and vaporize it, and the heat capacity of the filler and the decrease of the liquid ozone by the filler suppress the chain ozone decomposition due to the vaporization of the liquid ozone. As a result, it is possible to generate stable liquid ozone and to eliminate the possibility of destruction of the apparatus.

Hereinafter, a preferred embodiment of an ozone concentrator according to the present invention will be described with reference to the accompanying drawings. In the drawings, the same or corresponding elements are denoted by the same reference numerals, and redundant description is omitted.

[First embodiment]
FIG. 1 is a schematic configuration diagram showing a high-concentration ozone gas generation apparatus equipped with an ozone concentrator according to the first embodiment of the present invention, and FIG. 2 is a cooling unit, a liquid seal pipe of the ozone concentrator in FIG. It is a schematic block diagram which shows a vaporization part, and the high concentration ozone gas production | generation apparatus of this embodiment is high concentration ozone gas (generally the volume ratio of ozone is about 10% or more) used for formation of the oxide film of a semiconductor manufacturing apparatus etc., for example It is an apparatus capable of continuously generating this high-concentration ozone gas.

  As shown in FIG. 1, the high-concentration ozone gas generation apparatus 200 includes an ozonizer 10 that generates ozone gas (a volume ratio of ozone is about 10%), a cooling unit 1, and a vaporization unit 2, and concentrates ozone gas from the ozonizer 10. And an ozone concentrator 100 that generates high-concentration ozone gas.

  The ozonizer 10 generates ozone gas (the volume ratio of ozone is about 10%) based on oxygen or air introduced through the pipe 27.

  The cooling means 1 cools the ozone gas from the ozonizer 10 and separates it into liquid ozone and non-condensed gas. The cooling means 1 includes a cryogenic refrigerator 4 that is connected to an ozonizer 10 and cools an introduction pipe 3 that introduces ozone gas from the ozonizer 10 to a cryogenic temperature.

  Here, a cryocooler is used as the cryogenic refrigerator 4, and the lower copper plate 4b and the upper copper plate 4c attached to the cryohead 4a of the cryocooler 4 are used as the cooling unit 4x to constitute the cooling unit 4x. The introduction pipe 3 is sandwiched between the copper plates 4b and 4c and cooled. Thus, the introduction pipe 3 between the copper plates 4b and 4c is a cooling pipe 3c for separating the ozone gas into liquid ozone and non-condensed gas.

  The cooling unit 4x cools the ozone gas in the cooling pipe 3c to a temperature lower than the boiling point of ozone (−111.9 ° C.) and higher than the boiling point of oxygen (−183 ° C.). It is separated into non-condensable gas mainly composed of Moreover, this cooling part 4x is provided with the extension part 4y extended to the vaporization part 2 side.

  The cooling pipe 3c is inclined downward from the inlet 3a to the outlet 3b in the cooling unit 4x, and liquid ozone is prevented from being stored in the cooling pipe 3c.

  A gas pipe 5 directed upward and a liquid seal pipe 6 directed downward are joined and connected to the outlet 3b of the cooling pipe 3c. The gas pipe 5 guides the non-condensed gas mainly composed of oxygen separated by the cooling pipe 3c upward from the outlet 3b. The gas pipe 5 has an outlet connected to the pipe 27 and returns the separated non-condensed gas to the ozonizer 10. Further, the gas pipe 5 is provided with a valve (pressure adjusting means) V1, and further connected with a pressure adjusting chamber 21 that secures a certain amount of capacity at a position closer to the cooling pipe 3c than the valve V1. A vacuum pump P is provided at a position closer to the pipe 27 than the valve V1. By controlling the valve V1 to open and operating the vacuum pump P, the non-condensed gas can be efficiently guided to the ozonizer 10.

  Here, by controlling the valve V1 to open and driving the vacuum pump P, the upstream side of the gas pipe 5 from the valve V1 can be depressurized, thereby separating the boundary surface between the liquid ozone and the non-condensable gas. The pressure on 7 can be reduced. Conversely, if the valve V1 is controlled to be throttled or closed, the pressure upstream of the valve V1 of the gas pipe 5 can be increased, and the pressure on the separation boundary surface 7 can be increased.

  On the other hand, as shown in FIG. 1 and FIG. 2, the liquid seal pipe 6 connects the outlet 3b of the cooling pipe 3c and the inlet 2a of the vaporizing section 2, and is separated by the cooling section 3c and falls down from the outlet 3b. The liquid ozone seals the cooling pipe 3c and the gas pipe 5 side and the vaporizing part 2 side with the liquid ozone.

  Here, a U-shaped tube is used as the liquid-sealed piping 6, and the separation boundary surface 7 is located in the U-shaped tube 6 at a position slightly below the outlet 3b of the cooling tube 3c. The liquid surface 7a on the second side is configured to be positioned below the inlet 2a because the inlet 2a of the vaporizing section 2 is at a height higher than the separation boundary surface 7.

  The liquid sealing pipe 6 is filled with a filler 8 that develops a capillary force and guides liquid ozone in the liquid sealing pipe 6 into the vaporizing section 2. Here, the filler 8 is a wire mesh filler, and is configured to be densely configured to develop a capillary force and to enter the vaporizing unit 2 through the inlet 2a of the vaporizing unit 2.

  The filler 8 is not limited to a wire mesh filler, and may be, for example, a thin metal material or glass fiber that is densely arranged, for example, a fine silica gel or porous silica that is arranged in large numbers. Any filler may be used as long as it exhibits a capillary force. Then, the liquid seal pipe 6 is passed through the extension part 4y of the cooling part 4x, is sandwiched between the copper plates 4b and 4c, and is cooled by the extension part 4y.

  The liquid seal pipe 6 is provided with a capacitance level meter (first information acquisition means) 31 for acquiring information related to the liquid level of the separation boundary surface 7, and on the vaporization section 2 side. An electrostatic capacity type level meter (second information acquisition means) 32 for acquiring information related to the liquid level of the liquid surface 7a is provided. These capacitance type level meters 31 and 32 include probes 31a and 32a, current value measuring units 31b and 32b, and display units 31c and 32c.

  The capacitance type level meter 31 detects the liquid level of the separation boundary surface 7 by measuring the capacitance that changes depending on the upper and lower sides of the separation boundary surface 7. As shown in FIG. 2, the probe 31a of the capacitance type level meter 31 is provided on the separation boundary surface 7 side in the liquid seal pipe 6 and is provided so as to enter one side of the U-shaped tube, The capacitance that changes depending on the liquid level of the separation boundary surface 7 is detected by the probe 31a, and a current value corresponding to the capacitance is input to the external current value measurement unit 31b. Based on this current value, the separation boundary surface 7 level is detected and the result is displayed on the display unit 31c.

  The capacitance level meter 32 detects the liquid level of the liquid surface 7a by measuring the capacitance that changes depending on the upper and lower surfaces of the liquid surface 7a on the vaporization unit 2 side. The probe 32a of the capacitance type level meter 32 is provided on the liquid level 7a side in the liquid seal pipe 6 and is provided so as to enter the other side of the U-shaped tube, and changes depending on the liquid level of the liquid level 7a. The capacitance to be detected is detected by the probe 32a, a current value corresponding to the capacitance is input to the external current value measuring unit 32b, and the liquid level of the liquid surface 7a is detected based on this current value. Is displayed on the display unit 32c.

  The vaporization unit 2 is for vaporizing liquid ozone from the liquid seal pipe 6 and has a cylindrical body and closed in a bowl shape with a lower part as shown in FIGS. 1 and 2. In addition, an inlet 2a is provided at the lower end, and an upper portion is closed in a thin bowl shape, and an outlet 2b is provided at the upper end.

  As described above, the inlet 2a of the vaporizing section 2 is at a height equal to or higher than the separation boundary surface 7, and the wire mesh-like filler 8 entering the inside through the inlet 2a causes liquid ozone to flow into the vaporizing section 2 by capillary force. It arrange | positions so that it may spread along the bottom part inner surface of the said vaporization part 2 so that it may provide in a bottom part.

  An encircling wall 9 that encloses the lower portion is provided at the lower portion of the vaporizing unit 2. Room temperature air is passed through the surrounding wall 9 so as to heat and vaporize the liquid ozone provided to the bottom of the vaporizing unit 2. The heating method may be, for example, heating with a heater or the like.

  Above the lower part in the vaporization part 2, the filler 20 which enables passage of the high concentration concentrated ozone (high concentration ozone gas) produced | generated by vaporization is filled. Here, the filler 20 is a wire mesh filler, but may be, for example, a metal corrugated filler, silica gel, porous silica, or the like. Any filler may be used. In addition, the wire mesh filler 20 in the vaporization part 2 is comprised more roughly than the wire mesh filler 8 in the liquid seal piping 6. FIG. Incidentally, when many silica gels and porous silica are filled in both the liquid seal pipe 6 and the vaporization part 2, it is preferable to fill the vaporization part 2 with silica gel or porous silica larger than that in the liquid seal pipe 6. .

  As shown in FIG. 1, a high-concentration ozone gas pipe 11 having a valve V2 is connected to the outlet 2b of the vaporizing section 2, and a valve V3 and an ozone killer 13 are disposed upstream of the valve V2 of the high-concentration ozone gas pipe 11. Is connected. The high-concentration ozone gas pipe 11 is for supplying the high-concentration ozone gas generated in the vaporization unit 2 to the subsequent stage, and the exhaust pipe 12 is for decomposing the excessive high-concentration ozone gas into oxygen by the ozone killer 13 and releasing it to the atmosphere. belongs to.

  And from the cooling part 4x of the cooling means 1, the part on the cooling part 4x side in the introduction pipe 3, the part on the cooling part 4x side in the gas pipe 5, the liquid seal pipe 6, the vaporizing part 2, and the valve V2 in the high-concentration ozone gas pipe 11 The portion on the vaporization unit 2 side is housed in a container 14, and the container 14 is a vacuum heat insulating container whose inside is evacuated by driving a vacuum pump 15.

  The high-concentration ozone gas pipe 11 and the gas pipe 5 in the vacuum heat insulating container 14 are pressures that release the pressure in the pipe when the pressure becomes a set pressure or higher according to the pressure increase in the pipe when ozone decomposition occurs. Open valves 16 and 17 are respectively provided. Here, safety valves are used as the pressure release valves 16 and 17, but a release valve or the like that partially breaks and releases the pressure when the pressure becomes higher than the set pressure according to the pressure increase in the pipe may be used. . In the unlikely event that all of the liquid ozone is decomposed by ozone and the pressure release valves 16 and 17 release the pressure into the vacuum insulation container 14, the vacuum insulation container is set so that the pressure in the piping is equal to or lower than the supply pressure of the ozone gas. The volume of the gap in 14 is set.

  According to the high-concentration ozone gas generating apparatus 200 configured as described above, ozone gas is generated by the ozonizer 10 based on oxygen or air, and this ozone gas is introduced into the ozone concentrating apparatus 100 through the introduction pipe 3 to cool the cooling means 1. It is cooled to a very low temperature in the part 4x. This ozone gas is separated into liquid ozone and non-condensed gas mainly composed of oxygen in the vicinity of the outlet 3b of the cooling pipe 3c, and the non-condensed gas is returned to the ozonizer 10 through the gas pipe 5 to be used for generation of ozone gas. .

  Here, an operation method in the case of starting up the ozone concentrator 100 or restarting the operation after being stopped for a long time (initial state) will be described. In such an initial state, the liquid seal pipe 6 is filled with air, so that a good capillary force due to the filler 8 cannot be expressed, and the liquid seal pipe 6 has a cooling pipe 3c on the outlet 3b side. There is a risk that liquid ozone will accumulate more than specified (abnormal storage).

  Therefore, in the present embodiment, the liquid level of the separation boundary surface 7 is detected by the capacitance type level meter 31, and the valve V1 is controlled based on the detected level, thereby adjusting the pressure on the separation boundary surface 7, and the liquid The liquid ozone is pushed into the vaporizing section 2 while keeping the position constant so as not to exceed the specified level. Then, as shown in FIG. 3, the liquid ozone newly separated by the cooling pipe 3 c flows into the liquid seal pipe 6, and the separation boundary surface 7 is kept constant, while the amount of newly flowing liquid ozone is kept. The liquid level 7a advances to the vaporization part 2 side. When the valve V1 is controlled, it is performed while monitoring whether or not the separation boundary surface 7 is suddenly changed. In addition, the temperature of the vaporization part 2 at this time is set to a temperature higher by about 5 ° C. to 10 ° C. than the cooling pipe 3c so as not to flow backward due to a rapid temperature rise.

  As shown in FIG. 4, when the liquid level 7a has advanced to a position where it can be measured by the capacitance level meter 32, liquid ozone is discharged from the vaporizer 2 due to the difference between the pressure on the separation boundary surface 7 and the pressure on the liquid level 7a. In order to prevent spraying, the liquid surface 7a is advanced while gradually reducing the pressure difference. At this time, the valve V1 is controlled based on the liquid level of the liquid surface 7a detected by the capacitance level meter 32. Further, it is performed while monitoring whether or not the liquid levels of the separation boundary surface 7 and the liquid surface 7a are suddenly changed.

  When the liquid level 7a reaches the vicinity of the inlet 2a of the vaporizing unit 2 and the liquid sealing pipe 6 is filled with liquid ozone in a predetermined amount, the temperature of the vaporizing unit 2 is gradually increased so that the ozone concentration and pressure in the vaporizing unit 2 become as prescribed. To rise. At this time, there is a possibility that liquid ozone may be spouted if it is suddenly raised, so whether or not the liquid level of the separation boundary surface 7 and the liquid surface 7a is kept constant by the capacitance type level meters 31 and 32. The temperature of the vaporizing unit 2 is gradually increased while monitoring the above. Until the vaporization unit 2 can vaporize ozone as prescribed, the ozonizer prevents the newly generated liquid ozone from accumulating on the outlet 3b side of the cooling pipe 3c in the liquid sealing pipe 6. It is preferable to adjust the amount of ozone gas produced at 10.

  When the liquid sealing pipe 6 is filled with liquid ozone and the ozone concentration and pressure in the vaporization section 6 are as specified, the separation boundary surface 7 between the liquid ozone and the non-condensable gas is in the liquid sealing pipe 6 and is a cooling pipe. On the other hand, the liquid surface 7a on the vaporization part 2 side of liquid ozone is located below the inlet 2a. Then, according to the newly supplied liquid ozone, the liquid ozone in the liquid sealing pipe 6 proceeds to the vaporizing section 2 by the capillary force of the filler 8 and is well guided into the bottom of the vaporizing section 2 through the inlet 2a. And enter. The liquid ozone that has entered the bottom of the vaporizing unit 2 through the filler 8 is vaporized before being accumulated in the bottom of the vaporizing unit 2 by heating with room temperature air to generate high-concentration ozone gas. Passes through the filler 20 and is discharged from the outlet 2b.

  And in this embodiment, the high concentration ozone gas whose volume ratio of ozone is near 100% is produced | generated. This high-concentration ozone gas is flowed to the high-concentration ozone gas pipe 11 when it is used in the latter stage, while the excess high-concentration ozone gas is flowed to the exhaust pipe 12 and decomposed into oxygen by the ozone killer 13 and then released to the atmosphere. The

  Even in normal times, the high concentration ozone is controlled while controlling the valve V1 so that the separation boundary surface 7 and the liquid surface 7a become predetermined based on the liquid level detected by the capacitance level meters 31, 32. Is generated. Further, in this normal time, newly generated liquid ozone is favorably guided into the vaporizing section 2 by the capillary force of the filler 8 in the liquid seal pipe 6.

  In addition, since the pressure adjustment chamber 21 connected to the gas pipe 5 has a certain capacity, even if the volume of the gas pipe 5 is small, a sudden change in pressure due to the control of the valve V1 is prevented. Has been.

  As described above, in the ozone concentrator 100 according to the present embodiment, the liquid sealing pipe 6 is filled with the filler 8 that develops the capillary force, so that the liquid ozone is absorbed by the capillary force of the filler 8. On the other hand, even if ozone decomposition occurs due to some trigger, the generated heat is absorbed by the heat capacity of the filler 8 in the liquid-sealed pipe 6 while being well guided to the vaporization section 2 and the filler. As a result of the amount of liquid ozone being reduced by 8, chain ozone decomposition due to vaporization of liquid ozone is suppressed. This makes it possible to generate stable liquid ozone and eliminate the possibility of damage to the apparatus.

  Further, since the capacitance level meters 31 and 32 are provided in the liquid sealing pipe 6, when the liquid sealing pipe 6 is filled with liquid ozone, the pressure on the separation boundary surface 7 of the liquid sealing pipe 6 is determined. It is possible to monitor whether or not the liquid level on the separation boundary surface 7 side of the liquid seal pipe 6 is suddenly changed due to excessive application of the liquid, and the liquid ozone liquid on the separation boundary surface 7 side of the liquid seal pipe 6 is monitored. Whether the liquid ozone on the separation boundary surface 7 side is flowing well into the liquid seal pipe 6 on the vaporization section 2 side, and can be monitored. Monitoring whether the liquid level of the liquid ozone on the part 2 side is abruptly fluctuated and whether the liquid level on the vaporizing part 2 side is kept constant when the liquid sealing pipe 6 is filled with liquid ozone. The separation boundary surface based on the liquid level detected in this way Therefore, the abnormal storage on the separation boundary surface 7 side and the discharge and discharge of liquid ozone at the vaporization unit 2 are prevented, thereby enabling stable generation of liquid ozone and liquid sealing. Damage due to abnormal decomposition of ozone applied to the pipe 6 is suppressed, and there is no possibility of destruction of the apparatus.

  Further, since the pressure on the separation boundary surface 7 can be adjusted by the control of the valve V1, it is possible to send liquid ozone into the liquid seal pipe 6 by increasing the pressure on the separation boundary surface 7. In addition, it is possible to keep the liquid level of the separation boundary surface 7 constant and prevent liquid ozone from being stored more than specified (abnormal storage) on the inlet side of the liquid seal pipe 6. Even if the pressure is excessively applied to the separation boundary surface 7, it is possible to prevent the discharge of liquid ozone in the vaporization unit 2 by reducing the pressure. As described above, abnormal storage on the separation boundary surface 7 side and ejection of liquid ozone at the vaporization unit 2 are prevented, thereby enabling stable generation of liquid ozone and ozone applied to the liquid sealing pipe 6. Damage due to abnormal decomposition of the device is suppressed and the possibility of destruction of the device is eliminated.

  In addition, since the pressure adjustment chamber 21 is connected to the gas pipe 5 to ensure a certain capacity, even if the volume of the gas pipe 5 is small, sudden pressure fluctuations due to the control of the valve V1 are prevented. Yes.

  Further, the pressure on the separation boundary surface 7 side and the pressure on the vaporization section 2 side are adjusted, and the liquid ozone is filled in the liquid sealing pipe 6 while gradually reducing the difference between these pressures. In this case, the abnormal storage and the discharge of liquid ozone in the vaporizing unit 2 are prevented, and stable generation of liquid ozone is enabled, and damage due to the abnormal decomposition of ozone applied to the liquid sealing pipe 6 is suppressed. There is no risk of destruction.

  Moreover, in this embodiment, there exist the following effects. That is, the separation boundary surface 7 between the liquid ozone and the non-condensable gas and the vaporizing section 2 are connected only by the liquid sealing pipe 6 that enables liquid sealing, and the liquid ozone exists in the liquid sealing pipe 6 and the separation boundary. The surface 7 is located in the liquid seal piping 6. For this reason, the amount of liquid ozone is greatly reduced as compared with the prior art. Therefore, ozonolysis and chain ozonolysis due to some trigger are suppressed, and the possibility of damage to the apparatus is eliminated.

  Further, since the inlet 2a of the vaporizing section 2 is at a height higher than the separation boundary surface 7 and the upper end of the filler 8 enters the inside through the inlet 2a of the vaporizing section 2, the liquid ozone vaporizes. Since it enters the vaporization part 2 by the capillary force of the filler 8 without entering the part 2 and vaporizes well, and thus the liquid ozone in the vaporization part 2 is very small, ozone caused by some trigger Decomposition and chain ozonolysis are suppressed, and the possibility of damage to the apparatus is further eliminated.

  In addition, since the vaporizer 2 is filled with a filler 20 that allows the passage of concentrated ozone, even if ozone decomposition occurs due to some trigger, the generated heat is generated by the filler 20 in the vaporizer 2. Absorbed by heat capacity. For this reason, chain | strand ozonolysis of the concentrated ozone in the vaporization part 2 is suppressed, and the possibility of damage of an apparatus is further eliminated.

  In addition, since the liquid sealing pipe 6 is cooled by the cooling means 1, ozone decomposition due to some trigger is suppressed, and even if ozone decomposition occurs due to some trigger, the generated heat is generated in the liquid sealing pipe 6 by the cooling means 1. Therefore, chain ozone decomposition due to vaporization of liquid ozone is suppressed. For this reason, the possibility of damage to the apparatus is further eliminated. In addition, if bubbles are generated due to the vaporization of liquid ozone in the liquid seal pipe 6, the capillary action of the filler 8 may be interrupted. However, since the liquid seal pipe 6 is cooled by the cooling means 1, the generation of bubbles is suppressed. Capillary action is supposed to work reliably.

  In addition, the cooling unit 4x, the liquid sealing pipe 6, the vaporization unit 2, and the pressure release valves 16 and 17 are accommodated in the vacuum heat insulating container 14, and all of the liquid ozone should be decomposed by ozone and the pressure release valves 16 and 17 are pressurized. Since the volume of the gap in the vacuum heat insulation container 14 is set so that the pressure in the pipe is equal to or lower than the supply pressure of the ozone gas when the gas is opened in the vacuum heat insulation container 14, the gas pressure during ozone decomposition is The pressure relief valves 16 and 17 are opened to the gaps in the vacuum heat insulating container 14 through the pressure relief valves 16 and 17, and the possibility of damage to the apparatus is further eliminated. Moreover, the cooling by the cooling means 1 and the heating in the vaporization part 2 are efficiently performed by the vacuum heat insulation state 14.

  Furthermore, the cooling pipe 3c that is cooled by the cooling section 4x of the cooling means 1 and connected to the liquid seal pipe 6 is inclined downward toward the connection section with the liquid seal pipe 6, that is, toward the outlet 3b. Further, liquid ozone is prevented from being stored in the cooling pipe 3c, and the possibility of damage to the apparatus is further eliminated.

[Second Embodiment]
FIG. 5 is a schematic configuration diagram showing a cooling unit, a liquid seal pipe, and a vaporization unit of a high-concentration ozone gas generation apparatus equipped with an ozone concentrator according to a second embodiment of the present invention. The difference between the second embodiment and the first embodiment is that the liquid level is detected by measuring the pressure proportional to the height of the liquid level instead of the capacitance level meters 31 and 32. This is the point where pressure type level meters 33 and 34 are provided.

  The lower measurement portion 33a of the differential pressure type level meter 33 is provided on the separation boundary surface 7 side in the liquid seal pipe 6 and is provided on the bottom portion on one side in the U-shaped pipe, and is proportional to the liquid level of the separation boundary surface 7. The pressure is measured and input to the external pressure detector 33c. The upper measurement unit 33b is provided in the gas pipe 6, measures the pressure applied to the separation boundary surface 7, and inputs the pressure to the external pressure detection unit 33c. The pressure detection unit 33c detects the liquid level of the separation boundary surface 7 based on these pressure differences, and displays the result on the display unit 33d.

  Further, the lower measurement part 34a of the differential pressure type level meter 34 is provided on the liquid level 7a side in the liquid seal pipe 6 and at the bottom on the other side in the U-shaped pipe, and is proportional to the liquid level of the liquid level 7a. The pressure is measured and input to the external pressure detector 34c. The upper measuring unit 34b is provided in the vaporizing unit 2, measures the pressure applied to the liquid level 7a, and inputs the pressure to the external pressure detecting unit 34c. The pressure detection unit 34c detects the liquid level on the separation boundary surface 7 based on these pressure differences, and displays the result on the display unit 34d.

  According to such 2nd Embodiment, the effect similar to 1st Embodiment can be acquired.

  The present invention has been specifically described above based on the embodiment. However, the present invention is not limited to the above embodiment. For example, in the above embodiment, the separation boundary surface 7 and the liquid surface are particularly preferable. Although it is set as the structure which measures the liquid level of 7a, you may detect the presence or absence of liquid ozone in the regulation position of the separation boundary surface 7 side and the vaporization part 2 side of the liquid seal piping 6. FIG.

It is a schematic block diagram which shows the high concentration ozone gas production | generation apparatus provided with the ozone concentration apparatus which concerns on the 1st Embodiment of this invention. It is a schematic block diagram which shows the cooling part, liquid sealing piping, and vaporization part of the ozone concentration apparatus in FIG. In FIG. 2, it is a schematic block diagram which shows a mode that the liquid level is progressing within liquid sealing piping. In FIG. 2, it is a schematic block diagram which shows a mode that the liquid level advanced to the position which can be measured with the level meter by the side of a vaporization part. It is a schematic block diagram which shows the cooling part, liquid sealing piping, and vaporization part of the high concentration ozone gas production | generation apparatus provided with the ozone concentration apparatus which concerns on the 2nd Embodiment of this invention.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Cooling means, 2 ... Evaporation part, 5 ... Gas piping, 6 ... Liquid sealing piping (liquid sealing part), 7 ... Separation boundary surface, 8 ... Filler, 10 ... Ozonizer, 21 ... Pressure adjustment chamber, 31 ... Static Capacitance type level meter (first information acquisition unit), 32 ... Capacitance type level meter (second information acquisition unit), 33 ... Differential pressure type level meter (first information acquisition unit), 34 ... Differential pressure type Level meter (second information acquisition unit), 100 ... ozone concentrator, 200 ... high-concentration ozone gas generator, V1 ... valve (pressure adjusting means).

Claims (6)

Cooling means for cooling the ozone gas generated by the ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensable gas;
A vaporization unit that heats and vaporizes the liquid ozone separated by the cooling means to obtain concentrated ozone;
A liquid seal portion for liquid-sealing between a separation boundary surface between the liquid ozone and the non-condensable gas and the vaporization portion;
A filler that fills the liquid seal part and develops capillary force;
First information acquisition means for acquiring information on the liquid level of the separation boundary surface;
An ozone concentrating apparatus comprising: a second information acquisition unit configured to acquire information related to a liquid level on the vaporization unit side of the liquid sealing unit.   2. The ozone concentrator according to claim 1, wherein the information acquisition means is a capacitance level meter that measures a capacitance that varies depending on a liquid level.   2. The ozone concentrator according to claim 1, wherein the information acquisition means is a differential pressure type level meter that measures a pressure proportional to the liquid level. Cooling means for cooling the ozone gas generated by the ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensable gas;
A vaporization unit that heats and vaporizes the liquid ozone separated by the cooling means to obtain concentrated ozone;
A liquid seal portion for liquid-sealing between a separation boundary surface between the liquid ozone and the non-condensable gas and the vaporization portion;
A filler that fills the liquid seal part and develops capillary force;
Pressure adjusting means for adjusting the pressure on the separation boundary surface;
An ozone concentrating device comprising: A gas pipe for deriving the non-condensable gas;
The liquid seal part and the gas pipe are respectively branched and connected to the outlet of the ozone flow path cooled by the cooling part of the cooling means,
The pressure adjusting means is provided for the gas pipe;
5. The ozone concentrator according to claim 4, wherein a pressure adjusting chamber is connected upstream of the pressure adjusting means of the gas pipe. Cooling means for cooling the ozone gas generated by the ozonizer to a temperature below the boiling point of ozone and separating it into liquid ozone and non-condensable gas;
A vaporization unit that heats and vaporizes the liquid ozone separated by the cooling means to obtain concentrated ozone;
A method for operating an ozone concentrating apparatus comprising: a liquid sealing portion that seals between a separation boundary surface between the liquid ozone and the non-condensable gas and the vaporizing portion;
Filling the liquid seal part with a filler that develops capillary force,
Operation of an ozone concentrator characterized by filling the liquid ozone into the liquid sealing part while adjusting the pressure on the separation boundary surface side of the liquid sealing part and the pressure on the vaporization part side of the liquid sealing part Method.

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