Glass raw material supply device and method for separating tanks in said glass raw material supply device

Abstract

To provide a glass raw material feeder capable of making a separation operation between a raw material feeding pipe and a tank be efficient, and to provide a method of separating the tank therefrom according to the glass raw material feeder.SOLUTION: A glass raw material feeder comprises: a tank for storing liquid glass raw material; a piping part for feeding the liquid glass raw material to a predetermined facility from the tank, that is detachably connected to the tank; a decompression part for decompressing an interior of the piping part; and a gas feeding part for feeding purge gas to the tank and the piping part in order to purge the liquid glass raw material. The gas feeding part comprises: a heating part for heating the purge gas; a first purge line for constituting a part of the piping part and purging an interior of raw material feeding piping detachably connected to raw material take-out piping of the tank with the purge gas; and a second purge line capable of purging the interior of the raw material feeding piping with the purge gas at a maximum flow rate smaller than a maximum flow rate of the purge gas introduced into the interior of the raw material feeding piping via the first purge line.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present disclosure relates to a frit supplying apparatus and a method for separating tanks in the frit supplying apparatus. [Background technology]

[0002] In various factories where fluids such as gases and liquids are used as raw materials, the fluids are often transported to the factory in containers such as tanks, and then transferred from the containers to the location of use by piping. Patent Document 1 discloses methods for removing residues from piping for transporting fluids, including a method of removing (purging) the residues in the piping with a carrier gas such as an inert gas, a method of heating the piping to gasify the residues and then sucking them out from the end of the piping with a pump, and a method of heating the piping to once seal a gas such as an inert gas in the piping, and then repeatedly sucking out the sealed inert gas and the gasified residue as a diluted gas from the end of the piping with a pump several times or more (batch purging).

[0003] Patent Document 2 is an invention related to a tank filled with liquid chemicals supplied from a chemical supply source, transported to a position where a chemical consuming apparatus is installed, and used to supply liquid chemicals to the chemical consuming apparatus, and discloses the structure of the connection between the chemical consuming apparatus and the tank, and the procedure for connecting / disconnecting the chemical consuming apparatus from the tank. Specifically, it describes that during the connection work, a seal gas is passed through a connecting pipe provided at the tank side connection to purge the inside of the chemical connection flow path and the gas connection flow path. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2001-108199 A [Patent Document 2] JP 2016-179853 A Summary of the Invention [Problem to be solved by the invention]

[0005] In the inventions disclosed in Patent Documents 1 and 2, when the tank is separated, an inert gas or the like is passed through the piping to remove any fluid remaining therein, thereby purging the tank. However, it takes a long time to completely remove the remaining fluid and enable separation, resulting in a large consumption of purge gas. In particular, in winter, the temperature is low, so the fluid in the piping is less likely to vaporize, and it may take even longer to completely remove the liquid.

[0006] The present disclosure has been made in view of the above facts, and aims to provide a frit supplying apparatus and a method for separating a tank included in the frit supplying apparatus, which can improve the efficiency of the work of separating a frit supplying pipe from a tank. [Means for solving the problem]

[0007] A glass raw material supplying apparatus according to one embodiment of the present disclosure includes: A frit supply device for supplying liquid frit, comprising: a tank for containing the liquid glass frit therein; A piping section that is detachably connected to the tank and supplies the liquid glass frit from the tank to a predetermined facility; A pressure reducing section that reduces the pressure inside the piping section; a gas supplying unit for supplying a purge gas to the tank and the piping unit in order to purge the liquid glass frit; Equipped with The tank is a raw material extraction pipe connected to the piping portion, which extracts the liquid glass raw material from the tank and supplies the liquid glass raw material to the piping portion; a gas introduction pipe for introducing the purge gas into the tank; having The gas supply unit includes: A heating unit that heats the purge gas; a first purge line that constitutes a part of the piping section and that purges a raw material supply pipe that is detachably connected to the raw material unloading pipe with the purge gas; a second purge line capable of purging the inside of the raw material supply piping with the purge gas at a maximum flow rate that is smaller than a maximum flow rate of the purge gas introduced into the raw material supply piping through the first purge line; has.

[0008] A method for separating a glass frit tank according to an embodiment of the present disclosure includes the steps of: A method for separating a tank in the glass raw material supply device, comprising: a first step of purging the raw material supply pipe with the purge gas at a first flow rate through the first purge line; a second step of alternately repeating, after the first step, a step of purging the inside of the raw material supply pipe with the purge gas at a second flow rate lower than the first flow rate through the second purge line while heating the purge gas in the heating section, and a step of depressurizing the inside of the raw material supply pipe in the depressurizing section; a third step of disconnecting the tank from the raw material supply pipe after the second step; Includes. Effect of the Invention

[0009] According to the above disclosure, the efficiency of the work of disconnecting the raw material supply pipe from the tank can be improved. [Brief description of the drawings]

[0010] [Figure 1] FIG. 1 is a schematic diagram showing a glass raw material supply device in an embodiment of the present disclosure. [Diagram 2] 2 is a flowchart showing a process of separating the tanks in the glass raw material supplying apparatus of FIG. 1. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] Description of the embodiments of the present disclosure First, the embodiments of the present disclosure will be listed and described. A glass raw material supplying apparatus according to one embodiment of the present disclosure includes: (1) A frit supply device for supplying liquid frit, comprising: a tank for containing the liquid glass frit therein; A piping section that is detachably connected to the tank and supplies the liquid glass frit from the tank to a predetermined facility; A pressure reducing section that reduces the pressure inside the piping section; a gas supplying unit for supplying a purge gas to the tank and the piping unit in order to purge the liquid glass frit; Equipped with The tank is a raw material extraction pipe connected to the piping portion, which extracts the liquid glass raw material from the tank and supplies the liquid glass raw material to the piping portion; a gas introduction pipe for introducing the purge gas into the tank; having The gas supply unit includes: A heating unit that heats the purge gas; a first purge line that constitutes a part of the piping section and that purges a raw material supply pipe that is detachably connected to the raw material unloading pipe with the purge gas; a second purge line capable of purging the inside of the raw material supply piping with the purge gas at a maximum flow rate that is smaller than a maximum flow rate of the purge gas introduced into the raw material supply piping through the first purge line; has. According to this configuration, first, the majority of the liquid glass frit remaining in the raw material supply pipe is vaporized with a large flow rate of purge gas using the first purge line, and for the remaining liquid glass frit, the raw material supply pipe that is connected to the raw material take-out pipe of the tank is depressurized, and the raw material supply pipe is purged with heated purge gas through at least one of the first purge line and the second purge line. This can promote the vaporization of the liquid glass frit remaining in the raw material supply pipe, and can remove the liquid glass frit in a short time. As a result, the operation of disconnecting the raw material supply pipe from the tank can be made more efficient.

[0012] (2) an exhaust pipe for exhausting the purge gas used to purge the raw material supply pipe to a detoxification device; a hydrochloric acid concentration meter in the exhaust pipe for measuring a hydrochloric acid concentration of the purge gas; The device may further include: According to this configuration, it is possible to promptly check whether the liquid glass raw material has been reliably removed from the raw material supply pipe, thereby shortening the gas purging time.

[0013] A glass raw material supplying apparatus according to one embodiment of the present disclosure includes: (3) A method for separating a tank in the glass raw material supply apparatus according to the above (1) or (2), comprising the steps of: a first step of purging the raw material supply pipe with the purge gas at a first flow rate through the first purge line; a second step of alternately repeating, after the first step, a step of purging the inside of the raw material supply pipe with the purge gas at a second flow rate lower than the first flow rate through the second purge line while heating the purge gas in the heating section, and a step of depressurizing the inside of the raw material supply pipe in the depressurizing section; a third step of disconnecting the tank from the raw material supply pipe after the second step; Includes. According to this method, the liquid glass raw material remaining in the raw material supply pipe can be removed in a short time by repeatedly purging the inside of the raw material supply pipe with a heated purge gas and reducing the pressure of the raw material supply pipe.

[0014] (4) The first flow rate is 3 m 3 / h more than 30m 3 / hour or less, and the first step may be carried out for 30 minutes or more and 3 hours or less. According to this method, the liquid glass raw material remaining in the raw material supply pipe can be removed in a shorter time.

[0015] (5) When the hydrochloric acid concentration measured by a hydrochloric acid concentration meter provided in the glass raw material supplying apparatus becomes equal to or lower than a predetermined concentration, the second step may be terminated and the process may proceed to the third step. According to this configuration, it is possible to promptly check whether the liquid glass raw material has been reliably removed from the raw material supply pipe, thereby shortening the gas purging time.

[0016] DETAILED DESCRIPTION OF EMBODIMENTS OF THE DISCLOSURE A specific example of a frit supplying apparatus according to an embodiment of the present disclosure and a method for separating a tank included in the frit supplying apparatus will be described below with reference to the drawings. It should be noted that the present disclosure is not limited to these examples, but is intended to include all modifications within the scope and meaning equivalent to the claims, as defined by the claims.

[0017] First, with reference to FIG. 1, a glass raw material supplying apparatus 100 according to an embodiment of the present disclosure will be described. Fig. 1 is a schematic diagram showing an entire glass raw material supplying apparatus 100 according to the present embodiment (hereinafter, referred to as raw material supplying apparatus 100). As shown in Fig. 1, the raw material supplying apparatus 100 includes a tank (container) 1, a raw material supply piping section 2 (an example of a piping section), a pressure reducing section 3, a storage tank section 4, and a gas supplying section 5.

[0018] The tank 1 is transported by a transport means (e.g., a dedicated truck) (not shown) to an area where the raw material supply device 100 is installed. The tank 1 is composed of a tank body 10 and a connection unit 12 attached to the tank body 10. The tank body 10 has a hollow structure, and although not shown, is transported with the interior filled with liquid glass raw material. The liquid glass raw material is mainly a raw material for manufacturing optical fiber, and for example, SiCl4, GeCl4, etc. are used.

[0019] A connection unit 12 is attached to the upper surface of the tank body 10. The connection unit 12 includes a raw material discharge pipe 14, a gas introduction pipe 16, and a bypass pipe 18.

[0020] One end (the lower end in FIG. 1) of the raw material unloading pipe 14 is immersed in the liquid glass raw material (not shown in FIG. 1) filled in the tank body 10, and the other end (the upper end in FIG. 1) is connected to the raw material supply pipe section 2. Two opening and closing valves 140, 142 are provided on the part of the raw material unloading pipe 14 extending from the tank body 10.

[0021] One end of the gas introduction pipe 16 is inserted into the tank body 10. Two opening and closing valves 160 and 162 are provided on the portion of the gas introduction pipe 16 extending from the tank body 10.

[0022] The bypass pipe 18 connects a portion between the on-off valve 140 and the on-off valve 142 provided in the raw material discharge pipe 14 and a portion between the on-off valve 160 and the on-off valve 162 provided in the gas introduction pipe 16. That is, one end (the right end in FIG. 1) of the bypass pipe 18 is connected to the raw material discharge pipe 14, and the other end (the left end in FIG. 1) is connected to the gas introduction pipe 16. An on-off valve 180 is provided in the bypass pipe 18.

[0023] The raw material supply piping section 2 is a pipe for supplying liquid glass raw material from the tank 1 to the storage tank section 4. The raw material supply piping section 2 includes a raw material supply piping 20, an exhaust piping 22, and a vacuum piping 24. The raw material supply piping 20 has an upstream end detachably connected to the raw material discharge piping 14 of the tank 1, and a downstream end inserted into the storage tank section 4. As a result, the liquid glass raw material filled in the tank body 10 of the tank 1 is supplied to the raw material supply piping 20 through the raw material discharge piping 14, and further to the storage tank section 4. An opening and closing valve 26 is provided in the middle of the raw material supply piping 20. The opening and closing valve 26 is, for example, an air valve.

[0024] An exhaust pipe 22 is connected to the raw material supply pipe 20 upstream of the on-off valve 26. The downstream end of the exhaust pipe 22 is connected to the detoxification device 200. An on-off valve 28 is provided in the exhaust pipe 22. When the liquid glass frit remaining in the raw material supply pipe 20 is removed, the removed liquid glass frit is exhausted together with the gas through the exhaust pipe 22 to the detoxification device 200 and detoxified. The exhaust pipe 22 is provided with a hydrochloric acid concentration meter 80. The hydrochloric acid concentration meter 80 can measure the hydrochloric acid concentration of the gas passing through the exhaust pipe 22. For example, an air inlet is provided downstream of the on-off valve 28 of the exhaust pipe 22, and the concentration of hydrogen chloride gas generated by contacting the gas containing the liquid glass frit with moisture in the air is measured by the hydrochloric acid concentration meter 80. Therefore, the measurement value of the hydrochloric acid concentration meter 80 reflects the concentration of the liquid glass frit. The hydrochloric acid concentration meter 80 may also be capable of directly measuring the concentration of the liquid glass frit. In this case, the exhaust pipe 22 does not need to be provided with an air inlet.

[0025] An upstream end portion of the raw material supply pipe 20, that is, a portion (separation portion) 30 detachably connected to the connection unit 12 of the tank 1, is connected to a purge line 58a of the gas supply portion 5 described later.

[0026] A vacuum pipe 24 is connected between the part of the raw material supply pipe 20 to which the exhaust pipe 22 is connected and the on-off valve 26. The downstream end of the vacuum pipe 24 is connected to the exhaust pipe 22. An on-off valve 32 and a vacuum exhaust device (vacuum generator) 34 are provided in the vacuum pipe 24. The vacuum pipe 24, the on-off valve 32, and the vacuum exhaust device 34 constitute a pressure reduction section 3. The vacuum exhaust device 34 is used to suck the liquid glass raw material remaining in the raw material supply pipe 20. When the vacuum exhaust device 34 is operated with the on-off valve 32 open, the remaining liquid in the raw material supply pipe 20 is sucked and discharged to the decomposition device 200 via the vacuum pipe 24.

[0027] The storage unit 4 includes a storage tank 40 and a pipe 42. The storage tank 40 is capable of storing the liquid glass raw material supplied from the raw material supply pipe 20 therein.

[0028] The pipe 42 is a pipe for taking out the liquid frit stored in the storage tank 40 and supplying it to a processing equipment 300 (for example, an optical fiber manufacturing device). The pipe 42 is provided below the storage tank 40, and an opening / closing valve 44 and a pump 46 are provided in the middle of the pipe. The end of the pipe 42 downstream of the pump 46 is branched, and each downstream end is connected to the liquid frit processing equipment 300, 300. In FIG. 1, opening / closing valves 48a, 48b are provided at the branched parts 42a, 42b of the pipe 42, respectively. By operating the pump 46 with each opening / closing valve 44, 48a, 48b open, the liquid frit stored in the storage tank 40 is supplied to each processing equipment 300, 300.

[0029] The gas supply unit 5 is used to pressurize the inside of the tank body 10 of the tank 1 and to replace (purge) the inside of the raw material supply piping unit 2 with gas. The gas supply unit 5 has a gas supply source 50 and a gas piping unit 52. The gas supply source 50 supplies an inert gas to the tank body 10 and the raw material supply piping 20 of the raw material supply piping unit 2 via the gas piping unit 52. Hereinafter, the inert gas may also be referred to as a purge gas. As the inert gas, for example, nitrogen, argon, helium, etc. are used, and it is particularly preferable to use nitrogen from the standpoint of cost and safety.

[0030] The gas piping section 52 has a purge line 54 on the upstream side as viewed from the gas supply source 50, a heating section 56, and a purge line 58 on the downstream side. The upstream purge line 54 connected to the gas supply source 50 branches into two purge lines 54a and 54b. A flow meter 60 and an opening / closing valve 62 are provided in one purge line 54a (an example of a first purge line) of the two branched purge lines 54a and 54b. Similarly, a flow meter 64 and an opening / closing valve 66 are provided in the other purge line 54b (an example of a second purge line). The purge line 54a is configured so that the maximum gas flow rate of the purge gas is greater than that of the purge line 54b. The maximum gas flow rate of the purge gas passing through the purge line 54a is, for example, 3 m 3 / h more than 30m 3 / hour or less, and the maximum gas flow rate of the purge gas passing through the purge line 54b is, for example, 1 m 3 / hour more than 10m 3 / hour or less.

[0031] The downstream end of the purge line 54a and the downstream end of the purge line 54b are joined by a downstream purge line 58. A heating unit 56 is provided in the downstream purge line 58. The heating unit 56 is a device for heating the purge gas supplied from the gas supply source 50. The heating unit 56 is provided with, for example, a heater, and the purge gas that has passed through the heater is heated to about 25°C to 90°C.

[0032] An on-off valve 68 is provided downstream of the heating unit 56 of the downstream purge line 58. The purge line 58 branches into two purge lines 58a and 58b further downstream of the on-off valve 68. The downstream end of one of the purge lines 58a is connected to the raw material supply pipe 20 of the raw material supply pipe section 2 which is detachably connected to the raw material removal pipe 14 of the connection unit 12 attached to the tank body 10. That is, the downstream end of the purge line 58a is connected to the disconnection section 30 of the raw material supply pipe 20. The downstream end of the other purge line 58b is connected to the gas introduction pipe 16 of the connection unit 12. An on-off valve 69 is provided in the purge line 58a.

[0033] Furthermore, a vacuum purge line 70 branches off from the upstream purge line 54. An open / close valve 72 is provided on the vacuum purge line 70. The downstream end of the vacuum purge line 70 is connected to the vacuum exhaust device 34 provided on the vacuum piping 24.

[0034] In the raw material supplying device 100 thus constructed, a method of supplying liquid glass raw material from the tank 1 to the storage tank 40 of the storage tank section 4 through the raw material supply pipe 20 will be briefly described. First, the on-off valve 69 of the purge line 58a is closed, and one of the on-off valves 62 and 66 provided on the upstream purge line 54, the on-off valve 68 provided on the downstream purge line 58, and the on-off valves 160 and 162 provided on the gas introduction pipe 16 of the connection unit 12 are opened to supply purge gas from the gas supply source 50 into the tank body 10, and the inside of the tank body 10 is pressurized by the gas. Next, the on-off valves 140 and 142 provided on the raw material extraction pipe 14 of the connection unit 12 and the on-off valve 26 provided on the raw material supply pipe 20 are opened, and the liquid glass raw material taken out of the tank body 10 is supplied to the storage tank 40 through the raw material extraction pipe 14 and the raw material supply pipe 20. The supply amount of liquid glass frit to the storage tank 40, in other words, the remaining amount of liquid glass frit in the tank body 10, can be recognized, for example, by placing the entire tank 1 on a load cell (not shown) and measuring the change in the weight of the tank 1. When it is determined that the liquid glass frit in the tank body 10 is substantially all discharged and supplied to the storage tank 40, the opening and closing valve 180 provided in the bypass pipe 18 is opened, and the purge gas is also supplied into the raw material extraction pipe 14, so that the liquid glass frit remaining in the raw material extraction pipe 14 is returned to the tank body 10. Then, the opening and closing valve 160 provided in the gas introduction pipe 16 of the connection unit 12 and the opening and closing valve 140 provided in the raw material extraction pipe 14 of the connection unit 12 are closed. In addition, whether the liquid glass raw material in the tank body 10 has been substantially entirely discharged and supplied to the storage tank 40 may be judged by detecting a sudden increase in the measurement value of the flowmeter 60 when the opening / closing valve 62 provided in the upstream purge line 54 is opened, or a sudden increase in the measurement value of the flowmeter 64 when the opening / closing valve 66 is opened, in addition to measuring the change in the weight of the tank 1. Alternatively, a flowmeter for the liquid glass raw material may be provided in the raw material supply pipe 20, and the judgment may be made from the cumulative flow rate or the flow rate change.

[0035] Next, in the raw material supplying device 100, a method for removing the liquid glass raw material in the raw material supplying pipe 20 (a method for disconnecting the tank 1) when disconnecting the tank 1 from the raw material supplying pipe part 2 after the supply of the liquid glass raw material from the tank body 10 to the storage tank 40 is completed will be described below with reference to Figures 1 and 2. Figure 2 is a flow chart showing the process of disconnecting the tank 1 in the raw material supplying device 100.

[0036] First, in step S1 shown in Fig. 2, an operator closes the on-off valve 26 provided in the raw material supply pipe 20, the on-off valve 32 provided in the vacuum pipe 24, the on-off valve 66 provided in the purge line 54b, and the on-off valve 72 provided in the vacuum purge line 70, and supplies a purge gas from the gas supply source 50 toward the gas pipe section 52 while opening the on-off valve 28 provided in the exhaust pipe 22, the on-off valve 62 provided in the purge line 54a, and the on-off valve 68 provided in the purge line 58. Note that the on-off valve 69 of the purge line 58a is kept in a closed state while the liquid glass raw material is being supplied from the tank body 10 to the storage tank 40. As a result, the purge gas is supplied to the raw material supply pipe 20 through the upstream purge line 54, the purge line 54a, the downstream purge line 58 (purge line 58b), the on-off valve 162, the bypass pipe 18, and the on-off valve 142. As described above, the purge line 54a is configured to have a larger maximum gas flow rate than the purge line 54b. Therefore, the purge gas passing through the purge line 54a flows at a large flow rate (for example, 3 m 3 / h more than 30m 3 / hour or less) into the raw material supply pipe 20. At this time, the operator measures the gas flow rate of the purge line 54a by the flowmeter 60 provided in the purge line 54a, and adjusts the gas flow rate of the purge line 54a appropriately. The purge gas at a large flow rate supplied to the raw material supply pipe 20 purges (gas replaces) the liquid glass frit remaining in the raw material supply pipe 20 upstream of the opening and closing valve 26, and is sent to the decontamination device 200 side together with the purged liquid glass frit through the exhaust pipe 22. In step S1, the opening and closing valve 26 of the raw material supply pipe 20 and the opening and closing valve 32 of the vacuum pipe 24 are closed, so that the purge gas supplied to the raw material supply pipe 20 does not reach the raw material supply pipe 20 downstream of the opening and closing valve 26 or the vacuum pipe 24 downstream of the opening and closing valve 32. In step S1, a large flow rate of purge gas is supplied to the raw material supply pipe 20, so that most of the liquid glass raw material remaining in the raw material supply pipe 20 on the upstream side including the separation part 30 is replaced with gas (flushing process). The implementation time of the flushing process is, for example, 30 minutes or more and 3 hours or less.

[0037] Next, in step S2, the operator closes the open on-off valve 28 of the exhaust pipe 22 and the open on-off valve 62 of the purge line 54a, and opens the closed on-off valve 66 of the purge line 54b, to supply the purge gas from the gas supply source 50 to the gas pipe section 52. At this time, the on-off valve 26 of the raw material supply pipe 20, the on-off valve 32 of the vacuum pipe 24, and the on-off valve 72 of the vacuum purge line 70 are kept in a closed state as in step S1, and the on-off valve 68 of the purge line 58 is kept in an open state as in step S1. As a result, the purge gas supplied from the gas supply source 50 is supplied to the raw material supply pipe 20 through the purge line 54b and the downstream purge line 58. Since the maximum flow rate of the purge gas sent through the purge line 54b is smaller than that through the purge line 54a, the purge gas that has passed through the purge line 54b is supplied into the raw material supply pipe 20 at a flow rate smaller than that of the purge gas that has passed through the purge line 54a. At this time, the operator measures the gas flow rate of the purge line 54b using the flowmeter 64 provided on the purge line 54b, and adjusts the gas flow rate of the purge line 54b appropriately. In step S2, the on-off valve 26 of the raw material supply pipe 20 and the on-off valve 32 of the vacuum pipe 24 as well as the on-off valve 28 of the exhaust pipe 22 are closed, so that the small flow rate of purge gas supplied to the raw material supply pipe 20 through the purge line 54b pressurizes the raw material supply pipe 20 from the separation part 30 to the on-off valve 26 (pressurization process).

[0038] Next, in step S3, the operator closes the open valve 66 of the purge line 54b and the open valve 68 of the purge line 58, and opens the closed valve 28 of the exhaust pipe 22. At this time, the open valve 26 of the raw material supply pipe 20, the open valve 32 of the vacuum pipe 24, the open valve 62 of the purge line 54a, and the open valve 72 of the vacuum purge line 70 are kept closed as in step S2. As a result, the purge gas (gas containing liquid glass raw material) supplied into the raw material supply pipe 20 from the separation part 30 to the open valve 26 is exhausted from the exhaust pipe 22 to the decompression device 200. That is, the pressurized (tensioned) state in the raw material supply pipe 20 from the separation part 30 to the open valve 26 is released (depressurization process).

[0039] Next, in step S4, the operator closes the open valve 28 of the exhaust pipe 22, and opens the closed valve 32 of the vacuum pipe 24 and the open valve 72 of the vacuum purge line 70. At this time, the open valve 26 of the raw material supply pipe 20, the open valve 62 of the purge line 54a, the open valve 66 of the purge line 54b, and the open valve 68 of the purge line 58 are kept closed as in step S3. In this state, the operator supplies purge gas from the gas supply source 50 to the gas pipe section 52 and operates the vacuum exhaust device 34. As a result, the liquid glass raw material remaining in the raw material supply pipe 20 is sucked by the vacuum exhaust device 34, and the raw material supply pipe 20 is made negative pressure (pressure value of about -0.08 MPa). That is, the raw material supply pipe 20 from the separation section 30 to the open valve 26 is made vacuum (negative pressure) (vacuum drawing process). In this way, by making the raw material supply pipe 20 negative pressure, the boiling point of the liquid glass frit is lowered and evaporation is promoted. For example, by making the pressure value in the raw material supply pipe 20 about -0.08MPa, the boiling point of SiCl4 is lowered to about 15°C. The purge gas supplied from the gas supply source 50 reaches the vacuum exhaust device 34 through the vacuum purge line 70, and is sent to the decontamination device 200 through the vacuum pipe 24 downstream of the vacuum exhaust device 34 together with the purge gas (gas containing the liquid glass frit) in the raw material supply pipe 20 sucked by the vacuum exhaust device 34.

[0040] Next, in step S5, the operator closes the on-off valve 32 of the vacuum pipe 24 and the on-off valve 72 of the vacuum purge line 70, which have been opened, and opens the on-off valve 28 of the exhaust pipe 22, the on-off valve 66 of the purge line 54b, and the on-off valve 68 of the purge line 58, which have been closed. The on-off valve 26 of the raw material supply pipe 20 and the on-off valve 62 of the purge line 54a are kept closed as in step S4. In this state, the purge gas is supplied from the gas supply source 50 toward the gas pipe section 52, and heating of the purge gas by the heating section 56 provided in the purge line 58 is started. As a result, the purge gas that has reached the heating section 56 via the purge line 54b is supplied to the raw material supply pipe 20 in a state in which it has been heated by the heating section 56 to about 25°C to 90°C (heated gas purge process). Purging the raw material supply pipe 20 with a purge gas (e.g., N2 gas) heated to about 25°C to 90°C by the heating unit 56 can promote evaporation of the SiCl4 liquid remaining in the raw material supply pipe 20. In this way, the heated purge gas supplied to the raw material supply pipe 20 vaporizes the liquid glass frit remaining in the raw material supply pipe 20 from the separation unit 30 to the opening and closing valve 26, and is exhausted from the exhaust pipe 22 together with the glass frit gas toward the detoxification device 200.

[0041] Next, in step S6, the operator stops heating the purge gas by the heating unit 56 while keeping the on-off valve 28 of the exhaust pipe 22, the on-off valve 66 of the purge line 54b, and the on-off valve 68 of the purge line 58 open, and continues to supply the purge gas from the gas supply source 50 to the gas pipe unit 52. At this time, the on-off valve 26 of the raw material supply pipe 20, the on-off valve 32 of the vacuum pipe 24, the on-off valve 62 of the purge line 54a, and the on-off valve 72 of the vacuum purge line 70 are kept closed as in step S5. As a result, the purge gas that is not heated by the heating unit 56 is supplied to the raw material supply pipe 20 (unheated gas purging step). The unheated purge gas supplied to the raw material supply pipe 20 is exhausted from the exhaust pipe 22 to the decontamination device 200 while cooling the inside of the raw material supply pipe 20.

[0042] Next, in step S7, the worker measures the hydrochloric acid concentration in the exhaust pipe 22 using the hydrochloric acid concentration meter 80 provided in the exhaust pipe 22. Next, in step S8, the worker determines whether the measured hydrochloric acid concentration is equal to or lower than a predetermined threshold value. If it is determined that the hydrochloric acid concentration is not equal to or lower than the predetermined threshold value (No in step S8), the worker returns to the tensioning process in step S2 and repeats the processes from step S2 onward.

[0043] On the other hand, if it is determined that the hydrochloric acid concentration is equal to or lower than the predetermined threshold value (Yes in step S8), the operator separates the raw material supply pipe section 2 from the connection unit 12 of the tank 1 in step S9. Specifically, the operator closes the on-off valve 28 of the exhaust pipe 22, the on-off valve 162 and the on-off valve 142 of the connection unit 12, and opens the on-off valve 69 of the purge line 58a. Next, in the portion indicated by the symbol A in FIG. 1, the upstream end (separation section 30) of the raw material supply pipe 20 is separated from the downstream end of the raw material extraction pipe 14 of the connection unit 12, and the downstream end of the purge line 58b is separated from the upstream end of the gas introduction pipe 16 of the connection unit 12. After that, the separated tank 1 is carried out from the area where the raw material supply device 100 is installed by a transport means such as a dedicated truck. This completes the process of separating the tank 1 in the raw material supply device 100 according to this embodiment.

[0044] (Example) Incidentally, when the tank 1 is separated from the glass raw material supply device 100 after the liquid glass raw material (e.g., SiCl4 liquid) is sent from the tank 1 to the storage tank 40, if the SiCl4 liquid remains in the raw material supply pipe 20, the raw material supply pipe 20 will corrode. Therefore, it is necessary to purge the raw material supply pipe 20 with a purge gas (e.g., N2) before separating the tank 1, but conventionally, this purge process took about 8 hours.

[0045] Therefore, in this embodiment, according to the flow chart of FIG. 2, as shown in Table 1 below, a gas replacement process of the SiCl4 liquid remaining in the raw material supply pipe 20 with N2 gas was performed, and it was confirmed whether the residual SiCl4 liquid was removed. [Table 1]

[0046] As shown in Table 1, in this embodiment, the flushing process of step S1, the pressurizing process of step S2, the depressurizing process of step S3, the vacuum drawing process of step S4, the heated gas purging process of step S5, and the non-heated gas purging process of step S6 in Fig. 2 were carried out. After that, a test tube for inspection was attached to the detached part 30 of the raw material supply pipe 20, and the hydrogen chloride (HCl) concentration in the raw material supply pipe 20 was measured to confirm whether the SiCl4 liquid had dried up. As a result, the HCl concentration in the raw material supply pipe 20 was 0 ppm (0%). In this way, it was confirmed that the gas replacement process of the SiCl4 liquid with N2 gas can be completed in about 2 hours by carrying out the processes of steps S1 to S6.

[0047] In the vacuum drawing process of step S4, as described above, the residual SiCl4 liquid in the raw material supply pipe 20 is sucked, and the boiling point of the residual SiCl4 liquid is lowered by creating a negative pressure in the raw material supply pipe 20, thereby promoting the evaporation of the residual SiCl4 liquid. Next, in the heated gas purging process of step S5, as described above, the raw material supply pipe 20 is purged with N2 gas heated to 25°C to 90°C by the heating unit 56, thereby further promoting the evaporation of the residual SiCl4 liquid. In this way, it was confirmed that the time required to remove the residual SiCl4 liquid in the raw material supply pipe 20 was significantly shortened by going through the vacuum drawing process and the heated gas purging process. Note that the amount of N2 gas used can be reduced by performing the vacuum drawing process before the heated gas purging process. Specifically, the amount of N2 gas used was reduced by about 37 m 3 Approximately 25m from 3 can be reduced to.

[0048] Furthermore, when the time for each step was shortened compared to that in Table 1, it was confirmed that HCl was no longer detected in the raw material supply pipe 20 in about 1.5 hours after the start of the flushing step.

[0049] As described above, the raw material supplying device 100 for supplying liquid glass frit includes the tank 1 for storing liquid glass frit therein, the raw material supplying piping section 2 for supplying the liquid glass frit from the tank 1 to the storage tank section 4 by being detachably connected to the tank 1, the pressure reducing section 3 for reducing the pressure in the raw material supplying piping section 2, and the gas supplying section 5 for supplying the purge gas to the tank 1 and the raw material supplying piping section 2 to purge the liquid glass frit. The tank 1 has at least the raw material extracting piping 14 for extracting the liquid glass frit from the tank 1 and supplying it to the raw material supplying piping section 2 by being connected to the raw material supplying piping section 2, and the gas introducing piping 16 for introducing the purge gas into the tank 1. The gas supply unit 5 includes a heating unit 56 for heating a purge gas, a purge line 54a (an example of a first purge line) for purging the inside of the raw material supply pipe 20, which is a part of the raw material supply pipe unit 2 and is connected to the raw material removal pipe 14 in a detachable manner, with a purge gas, and a purge line 54b (an example of a second purge line) for purging the inside of the raw material supply pipe 20 with a purge gas at a maximum flow rate lower than the maximum flow rate of the purge gas introduced into the raw material supply pipe 20 through the purge line 54a. According to this configuration, the pressure inside the raw material supply pipe 20, which is detachable from the tank 1, is reduced, and heated purge gas is supplied to the raw material supply pipe 20 through either the purge line 54a or the purge line 54b, thereby accelerating vaporization of liquid glass frit remaining in the raw material supply pipe 20, particularly in the pipe interior near the detachment part 30, and on the inner surface of the opening / closing valve 142 and the opening / closing valve 162 on the detachment part 30 side, and the liquid glass frit can be removed in a short time. This makes it possible to improve the efficiency of the work when disconnecting the tank 1 and the raw material supply pipe section 2.

[0050] The raw material supplying apparatus 100 according to the present embodiment further includes an exhaust pipe 22 for exhausting the purge gas supplied into the raw material supplying pipe 20 to the detoxification apparatus 200, and a hydrochloric acid concentration meter 80 for measuring the hydrochloric acid concentration of the purge gas in the exhaust pipe 22. According to this configuration, it is possible to promptly check whether the liquid glass raw material has been removed from the raw material supplying pipe 20, particularly from the inside of the pipe near the separation part 30, and from the inner surfaces of the opening / closing valve 142 and the opening / closing valve 162 on the separation part 30 side, thereby shortening the gas purge time.

[0051] The method for disconnecting the tank 1 in the raw material supplying apparatus 100 according to the present embodiment includes a first step of purging the raw material supplying pipe 20 at a large flow rate (an example of a first flow rate) through the purge line 54a, a second step of alternately repeating a step of purging the raw material supplying pipe 20 at a small flow rate (an example of a second flow rate) through the purge line 54b while heating the purge gas in the heating unit 56 after the first step, and a step of depressurizing the raw material supplying pipe 20 by operating the vacuum exhaust device 34 of the depressurization unit 3, and a third step of disconnecting the tank 1 and the raw material supplying pipe 20 after the second step. By going through these steps, the liquid glass raw material remaining in the raw material supplying pipe 20 can be removed in a short time. The maximum flow rate of the purge gas purged through the purge line 54a is, for example, 3 m 3 / h more than 30m 3 / hour or less, and the implementation time of the first step is, for example, 30 minutes or more and 3 hours or less.

[0052] In the method for separating the tank 1 according to the present embodiment, when the hydrochloric acid concentration measured by the hydrochloric acid concentration meter 80 becomes equal to or lower than a predetermined concentration, the second step is terminated and the process proceeds to the third step. According to this method, it is possible to timely check whether the liquid glass raw material has been removed from the raw material supply pipe 20, thereby shortening the purging time. Alternatively, it is also possible to predetermine the number of times that the step of purging the raw material supply pipe 20 at a small flow rate (an example of a second flow rate) through the purge line 54b while heating the purge gas in the heating unit 56 in the second step and the step of depressurizing the raw material supply pipe 20 by operating the vacuum exhaust device 34 of the depressurization unit 3 are alternately repeated, without measuring the hydrochloric acid concentration, and to proceed to the third step after performing the steps a predetermined number of times.

[0053] Although the present disclosure has been described in detail and with reference to specific embodiments, it is clear to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the present disclosure. Furthermore, the number, position, shape, etc. of the components described above are not limited to the above embodiments, and can be changed to the number, position, shape, etc. that are suitable for implementing the present disclosure.

[0054] In the above embodiment, in the process of supplying liquid glass raw material from the tank 1 to the storage tank 4 and the process of purging gas into the raw material supply pipe 20, an example is described in which an operator manually opens and closes each of the opening and closing valves 26, 28, 32, 44, 48a, 48b, 62, 66, 68, 69, 72, 140, 142, 160, 162, and 180, but the opening and closing work of the opening and closing valves may be automated. [Explanation of symbols]

[0055] 1 Tank (container) 2. Raw material supply piping section (example of piping section) 3 Pressure reduction section 4 Storage tank section 5 Gas supply section 10 Tank body 12 Connection Unit 14 Raw material extraction piping 16 Gas introduction piping 18 Bypass piping 20 Raw material supply piping 22 Exhaust piping 24 Vacuum piping 26,28,32,44,48a,48b,62,66,68,69,72,140,142,160,162,180 Opening and closing valves 30 Separation section 34 Vacuum exhaust device (vacuum generator) 40 Storage Tank 42 Piping 42a Branch 42b Branch 46 Pump 50 Gas Supply Source 52 Gas piping section 54 (54a, 54b) Upstream purge line 56 Heating section 58(58a,58b) Downstream purge line 60,64 flow meter 70 Vacuum purge line 80 Hydrochloric acid concentration meter 100 Glass raw material supply device (raw material supply device) 200 Abatement equipment 300 Processing Facilities

Claims

1. A frit supply device for supplying liquid frit, comprising: a tank for containing the liquid glass frit therein; A piping section that is detachably connected to the tank and supplies the liquid glass frit from the tank to a predetermined facility; A pressure reducing section that reduces the pressure inside the piping section; a gas supplying unit for supplying a purge gas to the tank and the piping unit in order to purge the liquid glass frit; Equipped with The tank is a raw material extraction pipe connected to the piping portion, which extracts the liquid glass raw material from the tank and supplies the liquid glass raw material to the piping portion; a gas introduction pipe for introducing the purge gas into the tank; having The gas supply unit includes: A heating unit that heats the purge gas; a first purge line that constitutes a part of the piping section and that purges a raw material supply pipe that is detachably connected to the raw material unloading pipe with the purge gas; a second purge line capable of purging the inside of the raw material supply piping with the purge gas at a maximum flow rate that is smaller than a maximum flow rate of the purge gas introduced into the raw material supply piping through the first purge line; having an exhaust pipe for exhausting the purge gas used to purge the raw material supply pipe to a detoxification device; a hydrochloric acid concentration meter in the exhaust pipe for measuring a hydrochloric acid concentration of the purge gas; The glass raw material supply device further comprises:

2. A method for separating a tank in a glass raw material supplying apparatus according to claim 1, comprising: a first step of purging the inside of the raw material supply pipe with the purge gas at a first flow rate through the first purge line; a second step of alternately repeating, after the first step, a step of purging the raw material supply pipe with the purge gas at a second flow rate lower than the first flow rate through the second purge line while heating the purge gas in the heating section, and a step of depressurizing the raw material supply pipe in the depressurizing section; a third step of disconnecting the tank from the raw material supply pipe after the second step; 4. A method for isolating the tank, including:

3. The first flow rate is 3 m ３ / hour or more 30m ３ 3. The method according to claim 2, wherein the first step is carried out for 30 minutes or more and 3 hours or less.

4. 4. The method according to claim 2 or 3, wherein the second step is terminated and the third step is started when the hydrochloric acid concentration measured by the hydrochloric acid concentration meter provided in the glass raw material supply device becomes equal to or lower than a predetermined concentration.

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