JP4520372B2 - Refining cylinder and air or inert gas circulation purification device - Google Patents

Description

  The present invention relates to a purification cylinder for circulating air or an inert gas through a cylinder body, removing oxygen and moisture contained in the air or inert gas, and purifying, and air or inert gas provided with the purification cylinder. The present invention relates to a circulating purification apparatus.

  For example, in an organic EL display manufacturing factory, manufacturing is performed in an inert gas (for example, nitrogen) atmosphere in order to prevent oxidation of organic substances constituting the organic EL display and reaction with water. . That is, the manufacturing process of the organic EL display is performed in a metal chamber in an inert gas atmosphere.

  However, in order to make the inside of the metal chamber an inert gas atmosphere, the inert gas supplied into the metal chamber is directly discharged out of the metal chamber. For this reason, in recent years, the inert gas discharged | emitted out of a metal chamber is reused, and the consumption of an inert gas is restrained. In order to reuse the inert gas, an inert gas purifier is connected to the metal chamber via a pipe. And the exhaust gas discharged | emitted out of the metal chamber is supplied to a refiner | purifier via piping, and the inert gas refine | purified with this refiner | purifier is resupplied to a metal chamber (for example, refer patent document 1). .

The purification apparatus disclosed in Patent Document 1 includes a purification cylinder filled with an adsorbent and a catalyst, and further includes a heater for heating the adsorbent and the catalyst outside the purification cylinder. And the inert gas discharged | emitted out of the metal chamber is supplied to the refinement | purification cylinder of the said refiner | purifier via piping. In the refining cylinder, moisture and carbon dioxide in the inert gas are adsorbed by the adsorbent, and oxygen in the inert gas is captured by the catalyst. And the inert gas refine | purified by the removal of the water | moisture content, carbon dioxide, and oxygen in a refinement | purification apparatus is resupplied to a metal chamber via piping. The catalyst that traps oxygen and the adsorbent that adsorbs moisture and carbon dioxide are heated by a heater and further reduced and regenerated by supplying hydrogen gas.
JP-A-8-173748

  By the way, in the refinement | purification apparatus disclosed by patent document 1, the refinement | purification cylinder equips the outer side with the heater. For this reason, in the refining cylinder, it is necessary to provide an attachment structure for attaching the heater to the outside of the refining cylinder. As a result, the structure of the purification cylinder is very complicated, and the size of the purification cylinder is increased.

  The present invention has been made paying attention to such problems existing in the prior art, and the purpose thereof is a purification cylinder capable of reducing the size of the body and air or inertness provided with the purification cylinder. An object of the present invention is to provide a gas refining apparatus.

  In order to solve the above problems, the invention according to claim 1 is a purification in which air or inert gas is circulated through the cylinder body, oxygen and moisture contained in the air or inert gas are removed, and purification is performed. A cylinder having a catalyst layer filled with a catalyst having oxygen scavenging ability on the upstream side in the flow direction of the air or the inert gas in the cylinder body, and further downstream in the flow direction than the catalyst layer in the cylinder body An adsorbent layer filled with an adsorbent having water removing ability on the side, and further, heating means for heating the catalyst layer and the adsorbent layer is disposed in the cylinder body, and the heating means Temperature adjusting means for adjusting the heating temperature of the catalyst layer to be lower than the heating temperature of the adsorbent layer, and the catalyst layer, the adsorbent layer, and the heating means are contained in one cylinder body. The gist is that it was placed and placed.

  According to a second aspect of the present invention, in the purification cylinder according to the first aspect, the temperature adjusting means includes a cavity that separates the catalyst layer and the heating means along a radial direction of the cylinder main body, and an adsorbent layer. The distance between the cavity or the adsorbent layer separating the heating means and the heating means is zero, and the distance between the catalyst layer and the heating means along the radial direction of the cylinder body is: The gist is that it is set longer than the distance between the adsorbent layer and the heating means.

  According to a third aspect of the present invention, in the purification cylinder according to the second aspect, a partition cylinder is disposed inside the catalyst layer in the cylinder body, and a heater as the heating means is provided in the partition cylinder. The gist is that the cavity is provided between the circumferential surface of the heater that is accommodated and that faces the circumferential surface of the heater.

  According to a fourth aspect of the present invention, in the refining cylinder according to the third aspect, the cylinder main body has a cylindrical shape, and an accommodation cylinder is arranged in the cylindrical main body concentrically with the peripheral surface of the cylinder main body. The gist is that the heater is accommodated in the accommodating cylinder.

The gist of the invention described in claim 5 is that a gap for separating the catalyst layer and the adsorbent layer is provided between the catalyst layer and the adsorbent layer.
Invention of Claim 6 is connected to the supply destination of air or an inert gas through an outward path and an inward path, and is arrange | positioned between the said outward path and an inward path. The purification cylinder according to claim 1 is provided, the air or inert gas discharged from the supply destination is received through the return path, the air or inert gas is purified by the purification cylinder, and the purified air or inert gas is purified. The gist is that the active gas is re-supplied to the supply destination via the forward path and circulated.

  The invention according to claim 7 is the air or inert gas circulation purification apparatus according to claim 6, wherein an inlet side to the supply destination is provided in the forward path, and an outlet side from the supply destination is provided in the return path. A gist of the invention is that a bypass passage that bypasses the supply destination and communicates therewith is provided, and an open / close valve that can open and close the bypass passage is provided in the bypass passage.

  The invention according to claim 8 is the air or inert gas circulation purification apparatus according to claim 6 or claim 7, wherein the air or inert gas discharged from the supply destination is supplied to the purification cylinder; Recirculation of air or inert gas purified in the purification cylinder to the supply destination is performed using a circulation pump, and the circulation pump and the purification cylinder are in a case where both front and rear surfaces are configured to be opened and closed by a closing member. The refining cylinder is disposed on the rear side of the case, the circulation pump is disposed on the front side of the case, and an operator performs work on the front side of the case. Is the gist.

  The invention according to claim 9 is the air or inert gas circulatory purification apparatus according to any one of claims 6 to 8, wherein the inlet side to the supply destination in the forward path is the above-described supply side. An atmospheric pressure replacement line for replacing the inside of the supply destination from the inert gas atmosphere to the atmospheric pressure atmosphere is connected, and a discharge mechanism for discharging the inert gas discharged from the supply destination is provided in the return path. It is a summary.

  According to the present invention, the physique can be reduced in size.

  FIG. 1 shows an embodiment in which the present invention is embodied in a purification cylinder used for manufacturing an organic EL display and an inert gas circulation purification apparatus (hereinafter simply referred to as a circulation purification apparatus) equipped with the purification cylinder. Description will be given with reference to FIG.

  FIG. 1 shows an inert gas circulation purification system S. As shown in FIG. 1, the circulation purification system S includes a circulation purification device 11 and a glove box G as a supply destination of an inert gas (nitrogen in this embodiment). The glove box G is formed in a box shape formed by assembling a resin panel, for example. Further, in the circulation purification system S, the circulation purification device 11 is an outgoing pipe as an outgoing route for supplying the inert gas purified by the purification cylinder 31 (see FIG. 4) included in the circulation purification device 11 to the glove box G. A path 10a is provided. The circulation purification device 11 includes a return pipe 10 b as a return path for supplying the inert gas (exhaust gas) discharged from the glove box G to the purification cylinder 31.

  The circulation purification device 11 and the glove box G are connected via the forward conduit 10a and the return conduit 10b. In the circulation purification apparatus 11, the inert gas discharged from the glove box G is received by the purification cylinder 31 through the return pipe 10b, the inert gas is purified by the purification cylinder 31, and the purified inert gas is purified. Is re-supplied to the glove box G via the forward duct 10a and circulated. In the circulation purification system S, a circulation circuit that circulates the inert gas between the glove box G and the circulation purification device 11 is configured, and a closed circuit that eliminates contact of the inert gas with the atmosphere is configured. .

  Further, the circulation purification device 11 includes an inert gas supply source N as a supply source of the inert gas supplied to the glove box G, and a reducing gas to the purification cylinder 31 for reducing and regenerating the purification cylinder 31. And a reducing gas supply source H for supplying (hydrogen in this embodiment). Further, the circulation purification apparatus 11 includes an oxygen supply source D that supplies oxygen into the glove box G in order to replace the inside of the glove box G from an inert gas atmosphere to an atmospheric pressure atmosphere (oxygen concentration of about 20%). . In the circulation purification system S, the inert gas is supplied from the inert gas supply source N to the circulation purification device 11, and after the purification cylinder 31 is replaced by the inert gas, the inert gas is sent from the circulation purification device 11. It is supplied to the glove box G via the pipe line 10a. The inside of the glove box G is an inert gas atmosphere, and the manufacturing process of the organic EL display is performed in the glove box G.

  Then, circulation is performed in the direction in which the inert gas flows from the circulation purification device 11 to the glove box G through the forward conduit 10a and in the direction in which the inert gas flows from the globe box G to the circulation purification device 11 through the return pipeline 10b. The flow direction of the inert gas in the purification system S and the circulation purification apparatus 11 is used. In the circulating purification system S, the reducing gas is supplied from the reducing gas supply source H to the purification cylinder 31 of the circulation purification apparatus 11, and the purification cylinder 31 is reduced and regenerated by the reducing gas.

  Next, the circulation purification apparatus 11 will be described. FIG. 2 is a diagram schematically showing the connection between the internal configuration of the circulation purification apparatus 11 and the glove box G. As shown in FIG. 2, the circulation purification device 11 includes four (four systems) purification units 22 that purify the inert gas. In the circulatory purification apparatus 11 of the present embodiment, one glove box G is connected to one purification unit 22 via an outgoing line 10a and a return line 10b, and one purification unit 22 and the purification unit 22 are connected. One circulation circuit is constituted by one glove box G corresponding to the above, the forward duct 10a and the return duct 10b. And between the circulation purification apparatus 11 and the glove box G of this embodiment, four circulation circuits are comprised.

  The four purification units 22 of the circulation purification device 11 can be controlled by a controller 23, respectively. An operation panel (not shown) is connected to the controller 23, and an instruction can be transmitted to the controller 23 by operating the operation panel. In addition, a communication unit 24 is connected to the controller 23, and a command device 26 provided separately from the circulation purification device 11 is connected to the communication unit 24 via a communication cable 25. The circulation purification device 11 is configured so that the controller 23 controls the operation of each purification unit 22 based on the operation of the operation panel or an instruction from the command device 26 received by the communication unit 24 via the communication cable 25. It has become.

  Next, the internal structure of the circulation purification apparatus 11 will be specifically described with reference to FIGS. FIGS. 3A to 3C schematically show the internal structure of the circulation purification apparatus 11. Specifically, the purification cylinder 31, the filter F, the partition plate 29, and the circulation pump constituting the circulation purification apparatus 11. The arrangement of P is shown. In addition, in FIG. 3 (a)-(c), the pipe line, valve, etc. which comprise the circulation purification apparatus 11 are abbreviate | omitted.

  The circulation purification device 11 includes a case 27 made of a metal square box. 3A, the right side of FIG. 3B, and the lower side of FIG. 3C are the front side of the case 27, and the surface facing the front side of the case 27 is the rear surface of the case 27. To do. In the state where the circulation purification apparatus 11 is installed in the organic EL display manufacturing factory, the operation panel is disposed on the front surface of the case 27, and the operator stands so as to face the front surface of the case 27. Is to be operated. That is, in the circulatory refining device 11, work by an operator is performed on the front side of the case 27.

  The front side and the rear side of the case 27 are closed by attaching a closing plate 28 as a closing member, while the case 27 is opened by removing the closing plate 28 from the case 27. Therefore, FIG. 3A shows a state in which the closing plate 28 on the front side of the case 27 is removed and the front side of the case 27 is opened, and in FIG. 3B and FIG. The front and back both sides are closed by the closing plate 28.

  As shown in FIGS. 3A to 3C, in the case 27, two partition plates 29 that divide the case 27 into the front side and the rear side are disposed. In the case 27, eight purification cylinders 31 are arranged on the rear side of the case 27 with respect to the partition plate 29. A filter F is suspended and supported by a suspension member (not shown) on the front side of the case 27 with respect to the partition plate 29 in the case 27 and on the upper side in the case 27. This filter F is provided to remove impurities in the inert gas supplied to the glove box G. A circulation pump P is disposed in the case 27 on the front side of the case 27 with respect to the partition plate 29 and on the lower side in the case 27. The circulation pump P is used to supply the inert gas discharged from the glove box G to the purification cylinder 31 and to supply the purified inert gas purified by the purification cylinder 31 to the glove box G again. Is provided.

  Next, the refining cylinder 31 that constitutes a part of the refining unit 22 and is disposed between the forward duct 10a and the return duct 10b will be described in detail with reference to FIG. The refining cylinder 31 includes a cylindrical body 32 having a cylindrical shape with both upper and lower ends closed. A plurality of (three in this embodiment) spring members 33 are disposed on the inner bottom portion of the cylinder body 32, and two first screen members 341 and one filter 351 are disposed on the spring members 33. Are stacked. Then, impurities in the inert gas introduced into the purification cylinder 31 are removed by the first screen member 341 and the filter 351.

  A catalyst layer 36 filled with a catalyst is provided on the filter 351. Nickel is used as the catalyst. The nickel has a high oxygen scavenging ability, and further has the ability to capture a small amount of carbon monoxide, hydrogen, carbon dioxide, and the like. When an inert gas is supplied to the catalyst layer 36, oxygen, carbon monoxide, hydrogen, carbon dioxide and the like in the inert gas are captured by the catalyst layer 36.

  A second screen member 342 is disposed on the catalyst layer 36, and a partition cylinder 40 having a bottomed cylindrical shape is joined to the lower surface of the central portion of the second screen member 342. A central axis L <b> 2 of the partition tube 40 is located on the same axis as the central axis L <b> 1 of the tube body 32, and the partition tube 40 is disposed concentrically with the tube body 32. The partition tube 40 is disposed inside the catalyst layer 36. Therefore, the catalyst layer 36 is provided on the lower side of the cylinder body 32 in an annular region formed between the inner peripheral surface of the cylinder main body 32 and the outer peripheral surface of the partition cylinder 40. Further, an annular ring spacer 37 is disposed on the second screen member 342, and the ring spacer 37 is disposed concentrically with the cylinder body 32.

  Two third screen members 343 and a filter 352 are stacked on the ring spacer 37. Impurities in the inert gas are removed by the second and third screen members 342 and 343 and the filter 352. An adsorbent layer 38 filled with an adsorbent is provided on the filter 352. Synthetic zeolite is used as the adsorbent. The synthetic zeolite has the ability to remove water, and further has the ability to remove a small amount of carbon dioxide, carbon monoxide, and the like. When the inert gas is supplied to the adsorbent layer 38, moisture in the inert gas is adsorbed and removed by the adsorbent layer 38.

  The catalyst layer 36 and the adsorbent layer 38 have different thicknesses in the direction of the central axis L1 of the cylinder body 32. That is, the filling amount of the catalyst into the cylinder main body 32 is smaller than the filling amount of the adsorbent. The filling amount of the catalyst layer into the cylinder main body 32 and the filling amount of the adsorbent into the cylinder main body 32 can suitably exhibit the oxygen scavenging ability of the catalyst layer 36 and the water removal ability of the adsorbent layer 38. Is set.

  In the cylinder body 32, a ring spacer 37 is interposed between the catalyst layer 36 and the adsorbent layer 38, so that the catalyst layer 36 and the adsorbent layer 38 are connected to each other. A gap K is formed to be spaced apart in the stacking direction of 38 (in the direction of the central axis L1 of the cylinder main body 32). The inert gas that has passed through the catalyst layer 36 is diffused throughout the gap K and then supplied to the adsorbent layer 38. Three fourth screen members 344 are stacked on the adsorbent layer 38. The fourth screen member 344 removes impurities in the inert gas. The upper end portion of the cylinder body 32 on the uppermost fourth screen member 344 is closed by a lid member 39.

  A housing cylinder 41 having a bottomed cylindrical shape is joined to the central portion of the lid member 39, the upper end side being opened and the bottom end being provided with a bottom portion. The housing cylinder 41 is formed so that the outer diameter is smaller than the outer diameter of the partition tube 40, and the center axis L 3 of the housing tube 41 is collinear with the center axis L 1 of the tube body 32 and the center axis L 2 of the partition tube 40. It is provided so that it may be located in. That is, the storage cylinder 41 and the partition cylinder 40 are disposed concentrically with respect to the cylinder body 32. The storage cylinder 41 includes the lid member 39, the fourth screen member 344, the adsorbent layer 38, the filter 352, the third screen member 343, the ring spacer 37, and the second screen from the upper end to the lower end of the cylinder main body 32. The member 342 passes through and is inserted into the partition tube 40.

  In the housing cylinder 41, a heater 43 is housed as a heating means for heating the catalyst layer 36 and the adsorbent layer 38 from the inside. The heater 43 passes through the central portion in the radial direction, which is the inner side of the adsorbent layer 38, in the direction of the central axis L1 of the cylinder main body 32. The heater 43 is inserted into the catalyst layer 36 in the direction of the central axis L1 of the cylinder body 32.

  The peripheral surface of the heater 43 via the housing cylinder 41 and the inner peripheral surface of the catalyst layer 36 via the partition cylinder 40 facing the peripheral surface of the heater 43 are spaced apart by a certain distance. Therefore, an annular cavity T is interposed between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36. On the other hand, the distance between the peripheral surface of the heater 43 via the housing cylinder 41 and the inner peripheral surface of the adsorbent layer 38 facing the peripheral surface of the heater 43 is zero, and the peripheral surface of the heater 43 and the adsorbent The number of cavities interposed between the inner peripheral surface of the layer 38 is zero.

  A distance between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 is formed by forming the cavity T, and a distance between the peripheral surface of the heater 43 and the inner peripheral surface of the adsorbent layer 38. Is a temperature adjusting means for adjusting the heating temperature of the catalyst layer 36 by the heater 43 so as to be lower than the heating temperature of the adsorbent layer 38. In the present embodiment, due to the cavity T, the distance between the circumferential surface of the heater 43 and the inner circumferential surface of the catalyst layer 36 in the radial direction of the cylinder main body 32 is set so that the circumferential surface of the heater 43 and the adsorbent layer 38 are It is longer than the distance between the peripheral surface. Accordingly, the purification cylinder 31 is configured to adjust the heating temperature of the catalyst layer 36 by the heater 43 to be lower than the heating temperature of the adsorbent layer 38 by the cavity T. The size of the cavity T, that is, the distance between the circumferential surface of the heater 43 along the radial direction of the cylinder body 32 and the inner circumferential surface of the catalyst layer 36 facing the heater 43 is the oxygen of the catalyst layer 36. The value is set to a value suitable for exhibiting the capturing ability suitably.

  An introduction port 44 is provided on the lower peripheral surface of the cylinder main body 32 below the purification cylinder 31. The return pipe 10 b is connected to the introduction port 44, and the inert gas discharged from the glove box G is introduced into the cylinder main body 32 from the introduction port 44. In addition, a lead-out port 45 is provided in the lid member 39 above the purification cylinder 31. The outgoing port 10 a is connected to the outlet 45, and the inert gas that has passed through the catalyst layer 36 and the adsorbent layer 38 is led out of the cylinder body 32 from the outlet 45.

  Then, the flow of the inert gas introduced into the purification cylinder 31 from the introduction port 44 and passing through the purification cylinder 31 and led out from the outlet 45 is defined as a flow direction of the inert gas in the purification cylinder 31. In this case, a catalyst layer 36 is disposed on the upstream side in the flow direction within the cylinder body 32 of the purification cylinder 31, and an adsorbent layer 38 is disposed on the downstream side in the flow direction with respect to the catalyst layer 36. Further, the refined cylinder 31 is integrated with the catalyst layer 36, the adsorbent layer 38 and the heater 43 accommodated in one cylinder body 32.

  Next, the circuit configuration of the circulation purification apparatus 11 will be specifically described with reference to FIG. In addition, since four circulation circuits are comprised between the circulation purification apparatus 11 and the glove box G, and the circulation of the inert gas in each circulation circuit is the same, in FIG. 5, one circulation circuit is used. explain. Further, two purification cylinders 31 constituting the purification unit 22 of one circulation circuit, one purification cylinder 31 is a first purification cylinder 31A, and the other purification cylinder 31 is a second purification cylinder 31B.

  As shown in FIG. 5, in the return pipe 10b connected to the glove box G, the upstream side of the first and second refining cylinders 31A and 31B in the flow direction of the inert gas is a part of the return pipe 10b. Are branched into a first introduction pipe 12a and a second introduction pipe 12b. The first introduction pipe 12a is connected to the introduction port 44 of the first purification cylinder 31A, and the second introduction pipe 12b is connected to the introduction port 44 of the second purification cylinder 31B. Valves 52a and 52b are provided on the first introduction pipe 12a and the second introduction pipe 12b. In addition, a circulation pump P is provided on the return pipe 10b and on the upstream side in the flow direction of the inert gas rather than branching into the first introduction pipe 12a and the second introduction pipe 12b.

  The outlet 45 of the first purification cylinder 31A is connected to the first outlet 13a that constitutes a part of the outgoing line 10a, and the outlet 45 of the second purification cylinder 31B is connected to the outlet 45a. The second lead-out pipe 13b constituting the part is connected. Valves 53a and 53b are provided on the first outlet pipe 13a and the second outlet pipe 13b. The first lead-out pipe 13a and the second lead-out pipe 13b are converged on one outgoing pipe 10a and connected to the glove box G. The filter F and the flow rate sensor 60 are provided on the outgoing line 10a.

  A bypass passage 10c that bypasses and communicates with the glove box G is provided between the inlet side of the glove box G in the forward conduit 10a and the outlet side of the glove box G in the return conduit 10b. A valve 58 is provided on the passage 10c as an on-off valve that can open and close the bypass passage 10c. A valve 50 is provided on the outgoing pipe 10a and downstream of the bypass passage 10c in the flow direction of the inert gas. The valve 50 is provided on the return pipe 10b and more inert gas than the bypass passage 10c. A valve 51 is provided on the upstream side in the flow direction.

  Further, a pipe 10d is connected to the inert gas supply source N provided in the circulation purification apparatus 11, and the pipe 10d is branched into branch pipes 14a and 14b. The branch pipe 14a is connected to the first outlet pipe 13a, and the branch pipe 14b is connected to the second outlet pipe 13b. Valves 54a and 54b are provided on the branch pipes 14a and 14b, respectively. A filter 61, a valve 62, a regulator 63, and a check valve 64 are provided on the pipe line 10d. The downstream side in the flow direction of the inert gas from the branch point to the branch pipes 14a and 14b in the pipe 10d is connected to the first and second outlet pipes 13a and 13b of the next system to supply the inert gas. It is possible.

  Further, a pipe 10e is connected to the reducing gas supply source H provided in the circulation purification device 11, and the pipe 10e is branched into branch pipes 15a and 15b. The branch pipe 15a branched from the pipe 10e is connected to the first outlet pipe 13a, and the branch pipe 15b is connected to the second outlet pipe 13b. Valves 55a and 55b are provided on the branch pipes 15a and 15b, respectively. Further, a filter 65, a valve 66, a regulator 67, a check valve 68, and a throttle 69 are provided on the pipe line 10e, and a pressure sensor 70 is further connected. The downstream side in the flow direction of the reducing gas from the branch point to the branch pipes 15a and 15b in the pipe line 10e is connected to the first and second outlet pipes 13a and 13b of the next system so that the reducing gas can be supplied. .

  In addition, a pipe line 10f is connected to the oxygen supply source D provided in the circulation purification apparatus 11, and the pipe line 10f is the forward pipe line 10a and is upstream of the filter F in the flow direction of the inert gas. It is connected to the. A filter 75, a valve 76, a regulator 77, and a check valve 78 are provided on the pipe line 10f. The oxygen supply source D, the pipe line 10f, the filter 75, the valve 76, the regulator 77, and the check valve 78 constitute an atmospheric pressure replacement line M that replaces the inside of the glove box G from an inert gas atmosphere to an atmospheric pressure atmosphere. is doing.

  A first discharge pipe 16a is connected to the first introduction pipe 12a, and a second discharge pipe 16b is connected to the second introduction pipe 12b. The first discharge pipe 16a and the second discharge pipe 16b are discharge pipes. 16 is connected. The discharge pipe 16 is opened to the outside as a drain outlet. Valves 56a and 56b are provided on the first and second discharge pipes 16a and 16b, respectively. Further, a first pressure release pipe 17a is connected to the first introduction pipe 12a, and a second pressure release pipe 17b is connected to the second introduction pipe 12b, and the first pressure release pipe 17a and the second pressure release pipe are connected. The pipe 17 b is connected to the pressure release pipe 17. Valves 57a and 57b are provided on the first and second pressure release pipes 17a and 17b, respectively. A valve 72 is provided on the pressure release pipe 17, and a vacuum pump 71 is connected to the pressure release pipe 17. In addition, a pressure sensor 73 is provided downstream of the circulation pump P in the circulation direction of the inert gas in the return pipe 10b.

  Further, in the return pipe 10b, an exhaust pipe 80 is provided downstream of the circulation pump P in the flow direction of the inert gas and upstream of the branch point to the first introduction pipe 12a and the second introduction pipe 12b. It is connected. The exhaust pipe 80 is open to the outside of the circulation purification apparatus 11, and a valve 81 is provided on the exhaust pipe 80. In the return pipe 10b, the circulation pump P, the exhaust pipe 80, and the valve 81 constitute a discharge mechanism for discharging the inert gas in the glove box G.

  In the circulatory purification apparatus 11, the purification unit 22 includes first and second introduction pipes 12a and 12b, valves 52a and 52b on the first and second introduction pipes 12a and 12b, and first and second. The refining cylinders 31A and 31B, first and second outlet pipes 13a and 13b, and valves 53a and 53b on the first and second outlet pipes 13a and 13b are configured. Further, the forward duct 10a includes the first and second outlet pipes 13a and 13b, and the return duct 10b includes the first and second introduction pipes 12a and 12b.

  Subsequently, purification of the inert gas using the circulation purification device 11 in the circulation purification system S having the above-described configuration will be described. It is assumed that the circulation purification device 11 is operated by an operation panel provided in the case 27.

  First, when the power supply of the circulation purification apparatus 11 is turned on by operation of the operation panel, nitrogen replacement of the first purification cylinder 31A is performed. At this time, the valve 76 on the pipe line 10f is closed to stop the supply of oxygen from the oxygen supply source D, and the valve 66 on the pipe line 10e is closed to reduce from the reducing gas supply source H. Gas supply is stopped. Then, the valves 50 and 51 on the outgoing line 10a and the return line 10b, the valve 58 on the bypass path 10c, and the valve 81 on the exhaust pipe 80 are closed. Furthermore, valves 52a and 52b of the first and second introduction pipes 12a and 12b, valves 53a and 53b of the first and second outlet pipes 13a and 13b, valves 55a and 55b on the branch pipes 15a and 15b, The valves 56a and 56b of the first and second discharge pipes 16a and 16b are closed. Further, the valve 54a of the branch pipeline 14a is closed, and the valve 54b of the branch pipeline 14b is closed.

  Then, after the valve 72 on the depressurizing pipe 17 is opened, the vacuum pump 71 is driven, and when the valve 57a is opened, the first purification cylinder 31A is evacuated by the vacuum pump 71. Thereafter, the valve 54a on the branch pipeline 14a is opened, and the valve 54b on the branch pipeline 14b is closed. Further, the valves 57a and 57b on the first and second pressure release pipes 17a and 17b are closed, the valve 72 on the pressure release pipe 17 is closed, and the vacuum pump 71 is stopped.

  When the valve 62 on the pipe line 10d is opened, the inert gas is supplied from the inert gas supply source N toward the first purification cylinder 31A. When the inert gas from the inert gas supply source N passes through the filter 61 on the pipe line 10d, impurities are removed, and the inert gas stored in the inert gas supply source N by the regulator 63 at high pressure is removed. The pressure is reduced to a predetermined pressure. Further, the inert gas is supplied to the first purification cylinder 31A through the pipe line 10d, the branch pipe line 14a, the first outlet pipe 13a, and the outlet port 45, and the inside of the first purification cylinder 31A is replaced with nitrogen.

  Next, nitrogen replacement of the second purification cylinder 31B is performed. At this time, the valve 62 on the pipe line 10d is closed, and the supply of the inert gas is stopped. First, the valve 54a of the branch pipe 14a is closed, and the valve 54b of the branch pipe 14b is closed. Then, after the valve 72 on the pressure release pipe 17 is opened, the vacuum pump 71 is driven, and when the valve 57b is opened, the second purification cylinder 31B is evacuated by the vacuum pump 71. Thereafter, the valve 54b on the branch pipeline 14b is opened, and the valve 54a on the branch pipeline 14a is closed. Further, the valves 57a and 57b on the first and second pressure release pipes 17a and 17b are closed, the valve 72 on the pressure release pipe 17 is closed, and the vacuum pump 71 is stopped.

  When the valve 62 on the pipe line 10d is opened, the inert gas is supplied from the inert gas supply source N toward the second purification cylinder 31B. When the inert gas from the inert gas supply source N passes through the filter 61 on the pipe line 10d, impurities are removed, and the inert gas stored in the inert gas supply source N by the regulator 63 at high pressure is removed. The pressure is reduced to a predetermined pressure. Further, an inert gas is supplied to the second purification cylinder 31B through the pipe line 10d, the branch pipe line 14b, the second outlet pipe 13b, and the outlet port 45, and the second purification cylinder 31B is replaced with nitrogen.

  Next, in the circulation purification device 11, reduction regeneration of the first purification cylinder 31A is performed. At this time, the valve 76 on the pipe line 10f is closed and the supply of oxygen from the oxygen supply source D is stopped, and the valve 62 on the pipe line 10d is closed and the valve from the inert gas supply source N is closed. The supply of inert gas is stopped. The valves 50 and 51 on the forward pipeline 10a and the return pipeline 10b are closed, and the valve 58 on the bypass passage 10c is closed. Further, the valve 81 on the exhaust pipe 80 is also closed. Furthermore, valves 52a and 52b on the first and second introduction pipes 12a and 12b, valves 53a and 53b on the first and second lead-out pipes 13a and 13b, and valves 54a and 54b on the branch pipes 14a and 14b. Then, the valves 57a and 57b of the first and second depressurizing pipes 17a and 17b are closed. Further, the valve 55a of the branch pipe 15a is opened, the valve 55b of the branch pipe 15b is closed, the valve 56a of the first discharge pipe 16a is opened, and the second discharge pipe 16b is opened. The valve 56b is closed. The valve 72 on the pressure release pipe 17 is closed and the vacuum pump 71 is stopped.

  When the valve 66 on the pipe line 10e is opened, an inert gas is supplied from the reducing gas supply source H toward the first purification cylinder 31A. When the reducing gas from the reducing gas supply source H passes through the filter 65 on the pipe 10e, impurities are removed, and the reducing gas stored at a high pressure in the reducing gas supply source H by the regulator 67 reaches a predetermined pressure. Depressurized. Further, hydrogen is supplied to the first refining cylinder 31A through the pipe line 10e, the branch pipe line 15a, the first outlet pipe 13a, and the outlet port 45.

  When the first purification cylinder 31A is heated by the heater 43, the catalyst layer 36 and the adsorbent layer 38 are heated by the heater 43 in the first purification cylinder 31A. Here, a cavity T is interposed between the peripheral surface of the heater 43 via the housing cylinder 41 and the inner peripheral surface of the catalyst layer 36 via the partition cylinder 40. On the other hand, no cavity is interposed between the peripheral surface of the heater 43 via the housing cylinder 41 and the inner peripheral surface of the adsorbent layer 38, and the heater 43 and the adsorbent layer 38 are not separated from each other.

  For this reason, the heat generated from the heater 43 is hardly transmitted to the catalyst layer 36 by the cavity T, and the catalyst layer 36 is heated at a lower temperature than that directly heated by the heater 43. That is, the catalyst layer 36 is indirectly heated by the heat of the heater 43. On the other hand, the adsorbent layer 38 is directly heated by the heater 43 and heated at a temperature higher than that of the catalyst layer 36. Accordingly, the purification cylinder 31 can heat the catalyst layer 36 and the adsorbent layer 38 at different temperatures even when the single heater 43 is used.

  Then, due to the heat from the heater 43, the oxygen trapped in the catalyst layer 36 reacts with hydrogen to become water and leaves the catalyst. Further, water adsorbed on the adsorbent layer 38 is also released from the adsorbent. Thereafter, the water separated from the catalyst layer 36 and the adsorbent layer 38 is discharged through the first discharge pipe 16a and the discharge pipe 16 together with the reducing gas. As a result, the catalyst layer 36 and the adsorbent layer 38 of the first purification cylinder 31A are reduced and regenerated, and the oxygen scavenging ability of the catalyst layer 36 and the water removal ability of the adsorbent layer 38 are restored.

  Next, self-circulation of the inert gas is performed. At this time, the valve 76 on the pipe line 10f is closed to stop the supply of oxygen from the oxygen supply source D, and the valve 66 on the pipe line 10e is closed to reduce from the reducing gas supply source H. Gas supply is stopped. Further, the valve 62 on the conduit 10d is closed, and the supply of the inert gas from the inert gas supply source N is stopped.

  The valves 50 and 51 on the outgoing pipe 10a and the return pipe 10b are closed, and the valve 81 on the exhaust pipe 80 is also closed. Furthermore, valves 54a and 54b on the branch pipes 14a and 14b, valves 55a and 55b on the branch pipes 15a and 15b, valves 56a and 56b on the first and second discharge pipes 16a and 16b, The valves 57a and 57b of the second depressurizing pipes 17a and 17b are closed. Further, the valve 52a of the first introduction pipe 12a is opened, the valve 52b of the second introduction pipe 12b is closed, and the valve 53a of the first outlet pipe 13a is opened, so that the second outlet pipe The valve 53b of 13b is closed. The valve 72 on the pressure release pipe 17 is closed and the vacuum pump 71 is stopped.

  When the circulation pump P is driven, the inert gas in the first purification cylinder 31A is led out from the outlet 45 of the first purification cylinder 31A to the first outlet pipe 13a, and further passes through the filter F. It is supplied to the return pipe 10b through the bypass passage 10c. Thereafter, the inert gas is supplied from the first introduction pipe 12a to the first purification cylinder 31A, and is supplied to the return pipe 10b through the first outlet pipe 13a and the bypass passage 10c. That is, the inert gas is not circulated to the glove box G and is circulated through the first purification cylinder 31 </ b> A side in the circulation purification apparatus 11.

  Reduction and regeneration of the second purification cylinder 31B is performed in a state where the inert gas is self-circulating on the first purification cylinder 31A side. The valve 55b of the branch pipe 15b is opened, and the valve 56b of the second discharge pipe 16b is opened. Thereafter, similarly to the first purification cylinder 31A, the reducing gas is supplied from the reducing gas supply source H to the second purification cylinder 31B, and the second purification cylinder 31B is reduced and regenerated.

  Now, when the controller 23 is instructed to supply the inert gas to the glove box G in accordance with the operation of the operation panel while the inert gas is circulating in the first purification cylinder 31A side, on the bypass passage 10c. While the valve 58 is closed, the valve 50 on the outgoing line 10a and the valve 51 on the return line 10b are opened. Then, the inert gas that has circulated through the first refining cylinder 31A is supplied to the glove box G through the outgoing line 10a. The inside of the glove box G is made an inert gas atmosphere, and the inert gas discharged to the return pipe 10b is introduced into the first purification cylinder 31A from the inlet 44 through the return pipe 10b and the first introduction pipe 12a. Is done.

  The inert gas supplied from the inlet 44 to the first purification cylinder 31A is first introduced into the catalyst layer 36, oxygen contained in the inert gas in the catalyst layer 36, and a small amount of carbon monoxide, Hydrogen, carbon dioxide, etc. are removed. Further, the inert gas is led out to the gap K interposed between the catalyst layer 36 and the adsorbent layer 38 by the ring spacer 37 when it goes downstream in the flow direction in the first purification cylinder 31A. Then, the inert gas diffused throughout the gap K is led out to the adsorbent layer 38. Then, moisture in the inert gas and a small amount of carbon monoxide and carbon dioxide are adsorbed by the adsorbent.

  The adsorbent layer 38 also adsorbs water generated by a reaction between oxygen removed by the catalyst layer 36 and a reducing gas (hydrogen) introduced into the catalyst layer 36 during the reduction regeneration of the catalyst layer 36. Remove. Then, the inert gas purified through the first purification cylinder 31A is led out from the first purification cylinder 31A through the outlet 45. The inert gas led out of the first purification cylinder 31A is re-supplied to the glove box G through the forward line 10a after impurities are further removed by the filter F.

  When the inert gas is purified on the first purification cylinder 31A side for a predetermined period, the first purification cylinder 31A is reduced and regenerated, and at the same time, the inert gas purification is performed on the second purification cylinder 31B side. That is, the valve 52a on the first introduction pipe 12a is closed while the valve 52b on the second introduction pipe 12b is opened, and the valve 53a on the first outlet pipe 13a is closed. On the other hand, the valve 53b on the second outlet pipe 13b is opened. Then, the inert gas from the glove box G is introduced from the introduction port 44 to the second purification cylinder 31B via the return pipe 10b and the second introduction pipe 12b. The inert gas is purified by the second purification cylinder 31B, then led out of the second purification cylinder 31B, and re-supplied to the glove box G through the second outlet pipe 13b and the forward pipe path 10a.

  When the inert gas circulates through the second purification cylinder 31B, reduction regeneration of the first purification cylinder 31A is performed. In the same manner as described above, after the reduction and regeneration of the first purification cylinder 31A, the first purification cylinder 31A side is in a standby state until it is self-circulated.

  In the circulation purification device 11, the flow rate of the inert gas circulating in the circulation circuit is detected by the flow rate sensor 60 on the outgoing line 10a. When the flow rate of the inert gas becomes a predetermined amount or less, the inert gas is supplied from the inert gas supply source N under the control of the controller 23. In the circulation purification apparatus 11, the pressure in the circulation circuit (in the glove box G) is detected by the pressure sensor 73. When the pressure in the circulation circuit (in the glove box G) becomes equal to or higher than a predetermined pressure, the valve 57a on the first pressure release pipe 17a or the valve 57b on the second pressure release pipe 17b is controlled by the controller 23. Is opened, and the valve 72 is further opened. Further, when the vacuum pump 71 is driven under the control of the controller 23, the pressure in each circulation circuit is reduced.

  Further, when the inert gas in the glove box G is exhausted and the inside of the glove box G is set to an atmospheric pressure atmosphere, first, the valve 50 on the outgoing line 10 a is opened by the control of the controller 23. At the same time, the valve 51 on the return pipe 10b is opened. Further, when the valve 76 on the pipe line 10f and the valve 81 on the exhaust pipe 80 are opened and the circulation pump P is driven, the glove is supplied from the oxygen supply source D via the pipe line 10f and the forward line 10a. Oxygen (dry air) is supplied to the box G. At the same time, the inert gas in the glove box G is discharged to the atmosphere through the return pipe 10b and the exhaust pipe 80. Then, the oxygen concentration in the glove box G is about 20% by the atmospheric pressure replacement line M, and is replaced with atmospheric pressure.

According to the above embodiment, the following effects can be obtained.
(1) The refining cylinder 31 (first and second refining cylinders 31A and 31B) has a catalyst layer 36 and an adsorbent layer 38 in one cylinder main body 32, and further includes a catalyst layer 36 and an adsorbent layer 38. A heater 43 that can heat both layers 36, 38 from the inside is provided, and the catalyst layer 36, the adsorbent layer 38, and the heater 43 are accommodated in one cylindrical body 32. For this reason, for example, unlike the purification cylinder of the background art provided with a heater outside the refining cylinder 31, the structure of the refining cylinder 31 is simplified without the need for an attachment structure for attaching the heater 43 to the outside of the refining cylinder 31. And can be downsized.

  In the refining cylinder 31, the cavity T (temperature adjusting means) is interposed between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 that faces the peripheral surface of the heater 43. The distance between the surface and the inner peripheral surface of the adsorbent layer 38 facing the peripheral surface of the heater 43 was set to zero (temperature adjusting means). Therefore, the catalyst layer 36 is indirectly heated by the heat of the heater 43 by being separated from the heater 43, and the adsorbent layer 38 is directly heated by the heat of the heater 43, thereby heating the catalyst layer 36. The temperature can be lower than the temperature at which the adsorbent layer 38 is heated. Accordingly, even in a configuration in which different types of catalyst layers 36 and adsorbent layers 38 are provided in one cylindrical body 32 and the heater 43 is accommodated, the heater 43 suitably heats the catalyst layers 36 and the adsorbent layer 38. Thus, the reduction regeneration of the catalyst layer 36 and the adsorbent layer 38 can be suitably performed.

  (2) The circulation purification apparatus 11 (purification cylinder 31) and the glove box G are connected to each other by the forward duct 10a and the return pipeline 10b, and the inert gas discharged from the glove box G is purified by the purification cylinder 31 of the circulation purification apparatus 11. Then, the purified inert gas is re-supplied to the glove box G. Therefore, the inert gas supplied to the glove box G can be reused, and an increase in cost associated with mass consumption of the inert gas can be suppressed. Moreover, since the closed circuit of inert gas is comprised between the circulation purification apparatus 11 (purification cylinder 31) and the glove box G, the purity reduction of the inert gas by contact with inert gas and air | atmosphere is prevented. can do.

  (3) In the purification cylinder 31, a gap K is provided between the catalyst layer 36 and the adsorbent layer 38 along the stacking direction of both layers 36 and 38. For this reason, the inert gas that has passed through the catalyst layer 36 is diffused throughout the gap K and then supplied to the adsorbent layer 38. Therefore, for example, it is suppressed that the inert gas that has passed through the catalyst layer 36 is supplied to the adsorbent layer 38 as it is. That is, the inert gas after passing through the catalyst layer 36 is evenly supplied to the adsorbent layer 38 by passing through the gap K, so that the contact area between the adsorbent and the inert gas can be increased, The water adsorption ability in the agent layer 38 can be suitably exhibited.

  (4) The refining cylinder 31 is reduced and regenerated by supplying the reducing gas from the reducing gas supply source H. The water generated by the oxygen trapped in the catalyst layer 36 and the reducing gas (hydrogen) is adsorbed by the adsorbent layer 38. Therefore, it is not necessary to separately provide a mechanism for discharging the water generated when the refining cylinder 31 is reduced and regenerated, and the structure of the refining cylinder 31 can be simplified and the size can be reduced.

  (5) The circulation purification apparatus 11 includes the purification unit 22 including two purification cylinders 31 (the first purification cylinder 31A and the second purification cylinder 31B) as one system, and one glove box G is formed by one purification unit 22. The inert gas discharged from the plant is purified. For this reason, when the inert gas is purified in one purification cylinder 31 in the purification unit 22, reduction regeneration of the other purification cylinder 31 can be performed. Therefore, by using the two purification cylinders 31, the inert gas can be continuously purified, and the purified inert gas can be continuously supplied to the glove box G.

  (6) In the purified cylinder 31, the accommodation cylinder 41 is disposed in the cylinder body 32, and the heater 43 is accommodated in the accommodation cylinder 41. For this reason, it is possible to prevent the heater 43 from shaking as compared with the case where the heater 43 is directly suspended from the lid member 39 without providing the housing cylinder 41. Therefore, the distance between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 due to the shaking of the heater 43 can be prevented from being shifted and unevenness in the heating temperature of the catalyst layer 36 can be prevented. Further, an accommodation cylinder 41 is disposed on the central axis L <b> 1 of the cylinder body 32, and a heater 43 is accommodated in the accommodation cylinder 41. For this reason, the heater 43 can be disposed in the cylinder main body 32 along the central axis L <b> 1 of the cylinder main body 32. Therefore, the catalyst layer 36 and the adsorbent layer 38 can be provided concentrically around the heater 43, and uneven heating of the catalyst layer 36 and the adsorbent layer 38 can be suppressed.

  (7) In the refining cylinder 31, a partition cylinder 40 is disposed in the cylinder body 32, and a cavity T is partitioned between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 by the partition cylinder 40. Yes. For this reason, the cavity T can be reliably partitioned by the partition cylinder 40, and the heating temperature of the catalyst layer 36 can be reliably lowered than the heating temperature of the adsorbent layer 38. Furthermore, a partition tube 40 is disposed on the central axis L <b> 1 of the tube body 32, and a heater 43 is accommodated in the partition tube 40. For this reason, the cavity T and the catalyst layer 36 can be provided concentrically on the outer peripheral side of the heater 43. Therefore, uneven heating can be suppressed also in the catalyst layer 36 through the cavity T.

  (8) The inlet side to the glove box G in the forward conduit 10a and the outlet side of the glove box G in the return conduit 10b are connected by the bypass passage 10c. Then, the inert gas is supplied to the purification cylinder 31 via the bypass passage 10c, and the inert gas is self-circulated in the circulation purification apparatus 11 until immediately before the inert gas is supplied to the glove box G. . For this reason, the inert gas is always refine | purified by carrying out the self-circulation in the circulation purification apparatus 11. FIG. Therefore, when the supply of the inert gas to the glove box G is instructed, the purified inert gas can be supplied to the glove box G.

  (9) The circulatory refining device 11 contains a refining cylinder 31 and a circulating pump P in a case 27. In the case 27, a circulation pump P is disposed on the front side of the case 27, which is the side on which an operator works, and a purification cylinder 31 is disposed on the rear side of the circulation pump P. Therefore, in the circulation purification apparatus 11, the workability of the maintenance work of the circulation purification apparatus 11 can be improved by arranging the circulation pump P that is frequently maintained on the front side of the case 27. In addition, the filter F is also disposed in the case 27 on the front side of the case 27 that is the side on which the operator works. Therefore, in the circulatory purification apparatus 11, the workability of the maintenance work of the circulatory purification apparatus 11 can be improved by disposing the filter F that is frequently maintained on the front side of the case 27.

  (10) In the circulation purification apparatus 11, the oxygen supply source D was connected to the outgoing line 10a via the line 10f, and the atmospheric pressure replacement line M including the oxygen supply source D was connected. Further, an exhaust pipe 80 is connected to the downstream side in the inert gas flow direction from the circulation pump P on the return pipe 10 b, and a valve 81 is provided on the exhaust pipe 80. Then, while supplying oxygen from the oxygen supply source D to the outgoing line 10a, the valve 81 of the exhaust pipe 80 is opened and the circulation pump P is driven to replace the inert gas in the glove box G with oxygen. It can be an atmospheric pressure atmosphere. Therefore, the operator can easily enter and exit the glove box G.

  (11) In the refining cylinder 31, one heater 43 is accommodated in the cylinder main body 32, and the one heater 43 is disposed at the inner center part of the catalyst layer 36 and the adsorbent layer 38. For this reason, the structure of the refinement | purification cylinder 31 can be simplified compared with the case where the catalyst layer 36 and the adsorption agent layer 38 are heated using the several heater 43, and it contributes to size reduction of the refinement | purification cylinder 31. Can do.

In addition, you may change the said embodiment as follows.
A cavity T as temperature adjusting means may be interposed between the peripheral surface of the heater 43 and the inner peripheral surface of the adsorbent layer 38. In this case, the distance between the circumferential surface of the heater 43 and the inner circumferential surface of the catalyst layer 36 in the radial direction of the cylinder main body 32 is the distance between the circumferential surface of the heater 43 and the inner circumferential surface of the adsorbent layer 38. The heating temperature of the catalyst layer 36 is set to be longer than that of the adsorbent layer 38.

  As a temperature adjusting means, a heat conductive layer may be provided between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 and between the peripheral surface of the heater 43 and the inner peripheral surface of the adsorbent layer 38. . In this case, the heat conductivity of the heat conductive layer between the peripheral surface of the heater 43 and the inner peripheral surface of the catalyst layer 36 is the heat conductivity between the peripheral surface of the heater 43 and the inner peripheral surface of the adsorbent layer 38. The heating temperature of the catalyst layer 36 is made lower than the heating temperature of the adsorbent layer 38 by making it lower than the thermal conductivity of the feed.

In the case 27, the front and rear positions of the circulation pump P, the filter F, and the first and second refining cylinders 31A and 31B may be arbitrarily changed.
The circulation purification device 11 of the embodiment has a configuration including four purification units 22, but may be configured to include two or three purification units 22, or may be configured to include five or more purification units 22.

  In the refining cylinder 31, for example, heating means (for example, a heater 43) is provided between the outer peripheral surface of the catalyst layer 36 and the adsorbent layer 38 and the inner peripheral surface of the cylinder main body 32, and the catalyst layer 36 and the adsorbent layer 38 are You may heat from the outside.

  In the first and second refining cylinders 31A and 31B, the ring spacer 37 between the catalyst layer 36 and the adsorbent layer 38 may be deleted to eliminate the gap K. In this case, the catalyst layer 36 and the adsorbent layer A second screen member 342 is interposed between the two plates 38.

In the embodiment, nitrogen is embodied as the inert gas, but helium, argon, xenon may be used in addition to nitrogen, or air other than the inert gas may be used.
In the embodiment, synthetic zeolite is used as an adsorbent, but alumina or silica gel may be used in addition to synthetic zeolite.

The operation of the circulation purification device 11 may be performed based on an instruction from the command device 26.
○ Opening and closing doors as closing members may be provided on both the front and rear sides of the case 27.
○ The inert gas supply destination may be a metal chamber.

The block diagram which shows typically the circulation purification system of the inert gas of embodiment. The schematic diagram which shows the circulation purification apparatus of an inert gas. (A) is a front sectional view showing the inside of an inert gas circulation purification device, (b) is a side sectional view showing the inside of the inert gas circulation purification device, and (c) is an inside of the inert gas circulation purification device. FIG. Sectional drawing which shows the refinement | purification cylinder of embodiment. The circuit diagram of a circulation purification system.

Explanation of symbols

  K: Air gap, M: Atmospheric pressure replacement line, P: Circulation pump (discharge mechanism), T: Cavity as temperature adjusting means, 10a ... Outward path as forward path, 10b ... Return path as return path, 10c ... Bypass 11. Passage, 11 ... Air or inert gas circulation purification device, 27 ... Case, 28 ... Closing plate as a closing member, 31 (31A, 31B) ... Purification cylinder, 32 ... Cylinder body, 36 ... Catalyst layer, 38 ... Adsorption Agent layer, 40 ... partition cylinder, 41 ... storage cylinder, 43 ... heater as heating means, 53 ... valve as opening / closing valve, 80 ... exhaust pipe constituting discharge mechanism, 81 ... valve constituting discharge mechanism.

Claims (9)

A purifying cylinder that circulates air or inert gas through the cylinder body, removes oxygen and moisture contained in the air or inert gas, and purifies the cylinder.
The cylinder main body has a catalyst layer filled with a catalyst having oxygen scavenging ability on the upstream side in the flow direction of the air or the inert gas, and has a water removal ability downstream of the catalyst layer in the cylinder body in the flow direction. A heating means for heating the catalyst layer and the adsorbent layer is disposed in the cylinder body, and the catalyst layer is heated by the heating means. A temperature adjusting means for adjusting the temperature to be lower than the heating temperature of the adsorbent layer, and the catalyst layer, the adsorbent layer, and the heating means are accommodated and arranged in one cylinder body. Characterized purification cylinder. The temperature adjusting means includes a cavity that separates the catalyst layer and the heating means along the radial direction of the cylinder body, and a cavity that separates the adsorbent layer and the heating means or between the adsorbent layer and the heating means. The distance between the catalyst layer and the heating means along the radial direction of the cylinder body is set longer than the distance between the adsorbent layer and the heating means. The purification cylinder according to claim 1. A partition cylinder is disposed inside the catalyst layer in the cylinder main body, and a heater as the heating means is accommodated in the partition cylinder, and a catalyst layer facing the peripheral surface of the heater and the peripheral surface of the heater. The refinement | purification cylinder of Claim 2 with which the said cavity is provided between the surrounding surfaces. The cylinder main body has a cylindrical shape, and an accommodation cylinder is disposed concentrically with a peripheral surface of the cylinder main body in the cylinder body, and the heater is accommodated in the accommodation cylinder. The purification cylinder as described. The refinement | purification cylinder as described in any one of Claims 1-4 in which the space | gap which spaces apart this catalyst layer and an adsorbent layer is provided between the said catalyst layer and the said adsorbent layer. The purification cylinder according to any one of claims 1 to 5, wherein the purification cylinder is connected to a supply destination of air or an inert gas via a forward path and a return path, and disposed between the forward path and the return path. The air or inert gas discharged from the supply destination is received through the return path, the air or inert gas is purified by the purification cylinder, and the purified air or inert gas is purified via the forward path. A circulating and purifying apparatus for air or inert gas, which is re-supplied to a supply destination and circulated. A bypass passage is provided between the inlet side to the supply destination on the forward path and the outlet side from the supply destination on the return path, and bypasses the supply destination. The apparatus for circulating and purifying air or an inert gas according to claim 6, wherein an on-off valve capable of opening and closing the passage is provided. Supply of air or inert gas discharged from the supply destination to the purification cylinder and re-supply of air or inert gas purified by the purification cylinder to the supply destination are performed using a circulation pump, and the circulation pump The refining cylinder is housed in a case whose front and rear surfaces can be opened and closed by a closing member, the refining cylinder is disposed on the rear surface side of the case, and the circulation on the front side of the case The circulating purification apparatus for air or inert gas according to claim 6 or 7, wherein a pump is provided and an operator performs work on the front side of the case. An atmospheric pressure replacement line for replacing the inside of the supply destination from an inert gas atmosphere to an atmospheric pressure atmosphere is connected to the inlet side to the supply destination in the forward path, and the return path is discharged from the supply destination. The air or inert gas circulation purification apparatus according to any one of claims 6 to 8, wherein a discharge mechanism for discharging the inert gas is provided.

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