Storage device special for high-purity germanium tetrachloride for optical fiber

By using a double-layer tank structure, a refrigeration and temperature control device, and a nitrogen gas sealing system, the problem of purity reduction during the storage of germanium tetrachloride for optical fibers was solved, and stable storage and transportation of high-purity germanium tetrachloride were achieved.

CN120887115APending Publication Date: 2025-11-04YUNNAN CHIHONG INT GE CO LTD
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Patent Information

Application Number
CN202511328117.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-17
Publication Date
2025-11-04

AI Technical Summary

Technical Problem

Existing germanium tetrachloride storage devices for optical fibers are prone to contact with the outside environment during use and sampling, which leads to a decrease in product purity and affects quality.

Method used

It adopts a double-layer tank structure, with the inner tank and the outer tank forming a sandwich, combined with a refrigeration temperature control device and a nitrogen gas sealing system to ensure the temperature and humidity control of the storage environment and prevent the entry of outside air.

Benefits of technology

It effectively maintains the high purity of germanium tetrachloride, prevents purity reduction, and ensures stable product quality during storage and transportation.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a special storage device for high-purity germanium tetrachloride for optical fibers, which comprises a refrigeration temperature control device, an outer tank body, an inner tank body and a tank cover, a nitrogen cylinder cavity is arranged outside the inner tank body, and a nitrogen cylinder is arranged in the nitrogen cylinder cavity; a tank opening is formed in the top of the inner tank body; an air channel is formed in the outer top, close to the tank opening, of the inner tank body, an air hole communicated with the air channel and the interior of the inner tank body is formed in the inner tank body below the tank opening, and the air channel is communicated to a nitrogen cylinder in the nitrogen cylinder cavity through an air pipe; the inner tank body is arranged in the outer tank body and forms an interlayer, the refrigeration temperature control device is arranged in the refrigeration temperature control device cavity, and an evaporator copper pipe of the refrigeration temperature control device is arranged in the interlayer; and a product can be prevented from being in contact with the outside during taking and sampling.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical reagent storage equipment, in particular to a special storage device for high-purity germanium tetrachloride for optical fibers. BACKGROUND

[0002] Germanium tetrachloride (GeCl4) for optical fibers is a key chemical raw material in optical fiber manufacturing, mainly used for preparing germanium-doped optical fibers. Its core role is to add germanium elements in the core part of the optical fiber to increase the refractive index, thereby optimizing the signal transmission performance, such as achieving high bandwidth, low loss and wide wavelength range, etc. The material is widely used in communication, laser technology, optical fiber sensing and other fields.

[0003] The purity of germanium tetrachloride for optical fibers is extremely high, but due to the corrosive nature of germanium tetrachloride itself, and its tendency to produce toxic gases and decompose in water, there are strict requirements for its preparation, storage and transportation, especially the requirement for sealing is extremely strict, otherwise impurities may be produced and the requirements cannot be met. In the existing storage operation, corrosion-resistant stainless steel tanks are usually used as storage containers for storage in dry and low-temperature environments, but during use, when opening the storage tank to take out part of the raw material or when sampling the germanium tetrachloride in the tank, the tank opening or discharge opening will inevitably be in contact with the outside world. If the humidity of the environment is high at this time, impurities will be produced by the contact between the germanium tetrachloride and the outside world, affecting the product quality. SUMMARY

[0004] To solve or partially solve the problems in the related art, the present application provides a special storage device for high-purity germanium tetrachloride for optical fibers, which can avoid the product from contacting the outside world when taking and sampling.

[0005] The present application discloses a special storage device for high-purity germanium tetrachloride for optical fibers, comprising a refrigeration temperature control device, further comprising: An outer tank body is provided in two parts, namely an upper outer tank body and a lower outer tank body, which are detachably and tightly connected; the bottom of the lower outer tank body is structured with a baffle to divide it into a bottom refrigeration temperature control device cavity; and An inner tank body is provided with a nitrogen cylinder cavity on the outside, and a nitrogen cylinder is arranged in the nitrogen cylinder cavity; the top of the inner tank body is structured with a tank opening; a gas duct is arranged on the outer top of the inner tank body near the tank opening, and a gas hole is structured on the inner tank body below the tank opening to communicate the gas duct with the inside of the inner tank body; and the gas duct is connected to the nitrogen cylinder in the nitrogen cylinder cavity through a gas pipe. A tank cover is provided with a pump, the inlet of the pump is connected with an inner pipe inserted into the inner tank body, and an outer pipe is connected to the outlet of the pump, and a valve is arranged on the outer pipe; The inner tank is arranged in the outer tank and forms a sandwich, the refrigeration temperature control device is arranged in the refrigeration temperature control device cavity, and the evaporator copper pipe of the refrigeration temperature control device is in the sandwich.

[0006] Optionally, the baffle is a ring-shaped plate with a hollow portion, and mounting holes for placing the evaporator copper pipe are arranged on the plate.

[0007] Optionally, the sandwich is filled with a filler.

[0008] Optionally, the filler is a heat insulation and structural support filler.

[0009] Optionally, the upper outer tank and the inner tank are connected as a whole at the tank neck through a connecting filler.

[0010] Optionally, the air duct is arranged around the tank shoulder, and the air holes are arranged in multiple and are arranged obliquely upward.

[0011] Optionally, the inclination angle of the air holes is 5-15 degrees.

[0012] Optionally, a pressure sensor is embedded at the top of the tank mouth, an electromagnetic air valve is arranged on the air pipe, the pressure sensor and the electromagnetic air valve are connected to a first controller integrated with display and control, and the first controller is embedded on the outer tank.

[0013] Optionally, the connection part of the upper outer tank and the lower outer tank is configured with an upper mounting table and a lower mounting table that are embedded with each other, and the upper mounting table and the lower mounting table are fastened through screws after being embedded with each other.

[0014] Optionally, a corrosion-resistant sealing ring is configured at the bottom of the tank cover.

[0015] The technical scheme provided in the application can have the following beneficial effects: The device can avoid the influence of the environmental temperature and humidity on the purity of germanium tetrachloride when storing the germanium tetrachloride, can make the germanium tetrachloride be in a suitable storage environment through temperature control, and can avoid the entry of external air into the tank body after the tank body is opened through the nitrogen continuous air seal, so that the purity of the high-purity germanium tetrachloride for optical fibers is ensured, and the quality is not affected.

[0016] It should be understood that the above general description and the following detailed description are only exemplary and explanatory, and cannot limit the application. BRIEF DESCRIPTION OF DRAWINGS

[0017] The above and other objects, features and advantages of the present application will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings, in which like reference characters refer to like parts throughout the several views, and in which the exemplary embodiments of the present application are shown.

[0018] Figure 1 is a structural schematic diagram of an embodiment of the present application; Figure 2 is a sectional view of A-A of an embodiment of the present application; Figure 3 is a sectional view of B-B of an embodiment of the present application; Figure 4 is a sectional view of C-C of an embodiment of the present application; Figure 5 is an upper and lower bending structure of an evaporator copper tube of an embodiment of the present application; Figure 6 is a sectional view of installation of a nitrogen cylinder of an embodiment of the present application; Reference signs: 1, outer tank body; 11, upper outer tank body; 111, upper mounting table; 12, lower outer tank body; 121, baffle; 122, refrigeration temperature control device cavity; 123, mounting hole; 124, inner tank cavity; 125, lower mounting table; 2, inner tank body; 21, nitrogen cylinder cavity; 22, nitrogen cylinder; 23, threaded air valve; 24, electromagnetic air valve; 25, air pipe; 26, air passage; 27, air hole; 28, connecting filler; 29, pressure sensor; 210, tank opening; 3, tank cover; 31, pump; 32, inner tube; 33, outer tube; 34, valve; 4, filler; 5, refrigeration temperature control device; 51, evaporator copper tube; 6, sealing ring. DETAILED DESCRIPTION

[0019] Embodiments of the present application will be described in more detail by referring to the attached drawings. Although embodiments of the present application are shown in the drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments described herein. Rather, these embodiments are provided so that the present application is more thorough and complete, and the scope of the present application is fully conveyed to those skilled in the art.

[0020] It should be understood that, although the terms "first", "second", "third", etc. can be used in this application to describe various information, these information should not be limited to these terms. These terms are only used to distinguish information of the same type from each other. For example, the first information can also be referred to as the second information, and similarly, the second information can also be referred to as the first information without departing from the scope of the application. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise specifically limited.

[0021] In the description of the present application, it should be understood that the orientation or positional relationship indicated by the terms "length", "width", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation of the present application.

[0022] Unless otherwise specifically defined and limited, the terms "mounting", "connecting", "connecting", "fixing" and the like should be understood in a broad sense, for example, can be fixed connection, can also be detachable connection, or integral; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through intermediate medium; can be the internal communication of two elements or the interaction relationship between two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0023] In view of the above problems, the present application provides a high-purity germanium tetrachloride storage device for optical fibers, which is described in detail below in combination with the drawings.

[0024] As Figure 1 , Figure 2 , Figure 3 and Figure 4The illustrated high-purity germanium tetrachloride storage device for optical fibers includes a cooling and temperature control device 5 and an outer tank 1. The outer tank 1 is divided into two parts: an upper outer tank 11 and a lower outer tank 12, which are detachably and securely connected. The bottom of the lower outer tank 12 is divided by a baffle 121, creating a bottom cooling and temperature control device cavity 122. The outer tank 1 is designed with two detachably and securely connected parts to facilitate the manufacturing and use of the entire device. This structure can be modified according to specific needs, such as designing it as two mutually detachable and securely connected parts. The detachable connection in this application uses bolts for easy installation of the cooling and temperature control device 5. The cooling and temperature control device 5 in this application can be a conventional refrigerator cooling and temperature control device or system. In this application, the compressor, condenser, expansion valve, and other components required for refrigeration and temperature control are installed in the bottom refrigeration and temperature control device cavity 122. The evaporator is remade to accommodate the tank design of this application. The evaporator of this application is constructed using evaporator copper tube 51, that is, a copper tube is bent into an S-shape and then arranged in a ring along the inside of the tank. This application uses... Figure 5 The structure shown is bent upwards and downwards, then rolled into a cylindrical shape and inserted into the tank. In this way, the low temperature generated by the evaporator copper tube 51 in the refrigeration system is transferred to the tank, thereby achieving low-temperature control of the tank. During this process, appropriate controllers and intelligent control systems are set up as needed, and temperature sensors are placed in suitable locations to detect the temperature of the tank. The controller controls the entire refrigeration temperature control device to maintain the tank's interior at a suitable temperature for germanium tetrachloride storage.

[0025] The application also comprises an inner tank 2 for containing germanium tetrachloride, the outer part of the inner tank 2 is provided with a nitrogen cylinder cavity 21, and a nitrogen cylinder 22 is arranged in the nitrogen cylinder cavity 21; the top of the inner tank 2 is provided with a tank opening 210; a gas channel 26 is arranged on the outer top of the inner tank 2 close to the tank opening 210, and a gas hole 27 is arranged on the inner tank 2 below the tank opening 210 to communicate the gas channel 26 with the inside of the inner tank 2; the gas channel 26 is communicated to the nitrogen cylinder 22 in the nitrogen cylinder cavity 21 through a gas pipe 25; in this way, after the inner tank 2 is filled with germanium tetrachloride, on the one hand, the tank opening can be sealed by the nitrogen in the nitrogen cylinder 22 to prevent the germanium tetrachloride in the inner tank from volatilizing, and on the other hand, the nitrogen continuously released by the nitrogen cylinder 22 forms a gas wall seal at the tank opening 210, and at the same time, the nitrogen is continuously released to the outside to prevent the tank opening 210 from being opened or the inside germanium tetrachloride storage space from changing, so that the outside air enters the tank to reduce the purity of the germanium tetrachloride or cause pollution, especially to prevent the moisture in the air from entering the tank to cause chemical reaction with the germanium tetrachloride to reduce the purity of the germanium tetrachloride. Therefore, the nitrogen in the nitrogen cylinder 22 is compressed nitrogen, so that the nitrogen can be continuously supplied.

[0026] The application also comprises a sealable tank cover 3 which can be opened and closed, the tank cover 3 is provided with a pump 31, the inlet of the pump 31 is connected with an inner pipe 32 which is inserted into the inner tank 2, the outlet of the pump 31 is connected with an outer pipe 33, and the outer pipe 33 is provided with a valve 34. In this way, after the tank is sealed, the germanium tetrachloride in the tank can be pumped out by controlling the start of the pump 31, and the valve 34 is arranged mainly to prevent the purity of the germanium tetrachloride from being reduced due to the presence of water vapor in the distance from the pump 31 to the outlet of the pipe, and to prevent the presence of water vapor in the cavity of the pump itself due to the short distance between the outlet of the pump and the tank. In the process of use, the influence on the extraction of germanium tetrachloride can be reduced by reasonably controlling the start and stop of the pump 31 and the opening and closing of the valve 34, in this way, the valve 34 is a check valve, and the opening of the pump 31 generates a certain pressure to automatically open the valve 34, in this way, the backflow of the outside air into the pump body or the tank after the pump 31 stops is avoided.

[0027] In the application, the inner tank 2 is arranged in the outer tank 1 to form a sandwich, and the refrigeration temperature control device 5 is arranged in the refrigeration temperature control device cavity 122, and the evaporator copper pipe 51 of the refrigeration temperature control device 5 is arranged in the sandwich to form an evaporator, so that the temperature of the whole tank can be controlled to be in a suitable temperature range for the storage of germanium tetrachloride.

[0028] The application avoids the influence of environmental temperature and humidity on the purity of germanium tetrachloride when storing the germanium tetrachloride by letting the tank body have a temperature control nitrogen continuous air seal, and the germanium tetrachloride is kept in a proper storage environment through temperature control, and the tank body can still avoid the entry of external air when being opened through the nitrogen continuous air seal, thereby ensuring the purity of high-purity germanium tetrachloride for optical fibers and avoiding the reduction of the purity.

[0029] In an embodiment, in order to facilitate the placement and fixation of the evaporator copper pipe 51, the baffle 121 is an annular plate with a hollow in the middle to facilitate the installation and fixation of components such as compressors, condensers, expansion valves, etc., and the plate is provided with a mounting hole 123 for placing the evaporator copper pipe 51, which is fixed when passing through the mounting hole, and then connected with the expansion valve and the compressor. It should be noted that after the refrigeration temperature control device 5 is installed, a layer of heat insulation layer or a layer of heat insulation layer is preferably arranged between the inner tank body 2 and the top of the baffle 121 to separate the inner tank body 2 from the heat generated by the condenser. At the same time, an air outlet is needed to be opened on the outer tank body, and a fan is needed to be arranged to cool it if necessary. In this way, the storage temperature of the inner tank body 2 can be controlled as long as the equipment is powered on, so that the pure tank can be used for transportation while being stored. Of course, if possible, a filling material that simultaneously considers heat preservation or insulation and structural support, such as rock wool, glass wool or rigid polyurethane foam, is directly used as the filling material.

[0030] In an embodiment, since the inner tank body 2 is placed in the outer tank body 1 and forms a sandwich, the application is filled with a filling material 4 in the sandwich. On the one hand, it is to make the inner and outer tank bodies form a whole, and on the other hand, it is to make the inner and outer tank bodies have levels, mainly temperature levels. In this way, the filling material 4 is a heat insulation and structural support filling material. Specifically, a layer of heat insulation layer is arranged on the inner side of the outer tank body 1, and then a structural support filling material is poured into the space between the heat insulation layer and the inner tank body 2 to support the inner and outer tank bodies, so that the inner and outer tank bodies form a whole in mechanical structure and form levels in temperature change, which is convenient for the refrigeration temperature control device 5 to maintain the low temperature of the inner tank body 2 and also avoids the escape of temperature to the outer layer.

[0031] In an embodiment, in order to form the tank body and reduce components, the upper outer tank body 11 and the inner tank body 2 are connected at the tank neck through a connecting filling material to form a whole. For example, when the inner and outer tank bodies are both made of stainless steel, a piece of stainless steel can be used to connect the two into a whole by welding. When the inner and outer materials are inconsistent, the two can be connected into a whole by an intermediate filling material using a connecting material such as glue. In this way, installation is facilitated.

[0032] In one embodiment, the application uses nitrogen to seal the tank mouth 210, so the gas hole 27 is extremely critical, in the application, the gas channel 26 is arranged around the tank shoulder, preferably at the junction of the tank shoulder and the tank mouth corner, the gas channel 26 is connected with the inner tank body 2 as a whole by welding, and a connecting port is arranged at the position close to the nitrogen cylinder cavity 21 of the gas channel 26 as an interface for communication with the nitrogen cylinder. The gas hole 27 is arranged in multiple and inclined upward, and the inclination angle of the gas hole 27 is selected from 5 degrees to 15 degrees, and preferably 0 degree. In this way, after the germanium tetrachloride filling is completed, the liquid surface is just below the gas hole 27, and the multiple gas holes 27 blow out the other with a certain pressure to form a upward convex cone-shaped gas wall, and at the same time, due to the sealing of the bottom space, when the tank mouth 210 is opened, the excess other will escape outward, combined with the gas wall to prevent the external space from entering.

[0033] In one embodiment, after the sealing of the tank body cover with the tank cover 3 after the sealing of the gas seal is completed, the tank body cannot be filled with gas all the time, and the internal gas seal needs to reach the required pressure. When the tank cover 3 is opened, the gas seal is in operation, so the triggering condition is to judge the opening of the tank cover 3, and the condition can be converted into the change of the gas pressure in the tank body or the pressure change between the tank cover and the tank body. Therefore, the top of the tank mouth 210 is embedded with a pressure sensor 29, and a pressure sensor is also arranged in the gas channel 26. The gas pipe 25 is provided with an electromagnetic gas valve 24, and the two pressure sensors 29 and the electromagnetic gas valve 24 are connected to a first controller integrated with display and control, which is embedded on the outer tank body 1. In this way, when the pressure sensor in the gas channel 26 detects that the gas pressure in the tank body reaches the sealing requirement, the opening of the electromagnetic gas valve 24 is stopped, the nitrogen cylinder 22 is closed, and the tank body is normally sealed and stored; when the tank body is opened, the pressure between the tank cover 3 and the tank body changes, the internal space also changes, and the pressure also changes. The first controller controls the electromagnetic gas valve 24 to open a certain opening degree, and fills the nitrogen into the tank body to change; when the tank cover 3 is completely opened, the control gas controls the electromagnetic gas valve 24 to be completely opened at the moment to form a gas wall at the tank mouth 210 and prevent external air from entering the tank body.

[0034] In one embodiment, in order to facilitate the plug-in use of the nitrogen cylinder 22, such as Figure 6As shown, the nitrogen cylinder cavity 21 and the nitrogen cylinder 22 are both set as cylindrical shape, a cylindrical rotating groove with internal thread is set at the bottom of the nitrogen cylinder cavity 21, a connecting pipe is set at the bottom of the groove, a gas needle is set at the center of the groove bottom, and air holes are set around the gas needle and connected with the connecting pipe; the bottle mouth of the nitrogen cylinder 22 is provided with external thread and is screwed with the cylindrical rotating groove, the bottle mouth is provided with a needle guide valve like a basketball or a tire valve, when the nitrogen cylinder 22 is screwed in the cylindrical rotating groove, the needle guide valve is opened by the gas needle to release the gas in the nitrogen cylinder 22, and then the connecting pipe is connected to the electromagnetic valve 24 as an electrically controlled switch to control the release of nitrogen. A rotating handle is set at the bottom of the nitrogen cylinder 22, when the nitrogen cylinder 22 is inserted into the nitrogen cylinder cavity 21 and is opposite to the cylindrical rotating groove, the rotating handle is rotated to fix the nitrogen cylinder 22 and guide the nitrogen. A cavity cover is set outside the nitrogen cylinder cavity 21 to cover the entire nitrogen cylinder cavity 21.

[0035] In an embodiment, in order to facilitate the embedded connection of the upper outer tank body 11 and the lower outer tank body 12, an upper mounting table 111 and a lower mounting table 125 are arranged at the connection of the upper outer tank body 11 and the lower outer tank body 12, and the upper mounting table 111 and the lower mounting table 125 are embedded and fastened by screws after embedding.

[0036] In an embodiment, a corrosion-resistant sealing ring 6 is arranged at the bottom of the tank cover 3, which can be sealed after the tank cover 3 covers the entire tank body. The connection mode of the tank cover 3 and the tank body can be selected according to specific needs, such as threaded connection, external cover pressing, or plunger, etc.

[0037] In an embodiment, the use method of the high-purity germanium tetrachloride special storage device for optical fibers in the above-mentioned embodiment includes the following steps: S1: cleaning and drying each part of the device; S2: assembling the device, including the following steps: Step B1: assembling and fixing the refrigeration temperature control device 5 in the outer tank body 1; Step B2: assembling and fixing the upper outer tank body 11 and the inner tank body 2; Step B3: assembling the inner and outer tank bodies; Step B4: injecting the filler and fixing the tank body; S3: verifying and finally cleaning the assembled tank body: including the following steps: Step C1: electrical connection; Step C2: manual verification of inflation; Step C3: automatic verification of inflation; Step C4: air wall verification; Step C5: refrigeration temperature control verification; Step C6: pre-filling cleaning.

[0038] wherein, In step S1, the tank is mainly divided into two parts of the outer tank 1 which can be disassembled, the inner tank 2 which is integrally formed, and the tank cover 3. On the one hand, it is convenient for manufacturing and assembling, and on the other hand, it is convenient for cleaning the tank. The tank is in a disassembled state before cleaning. Before the tank is assembled, each part of the tank is cleaned separately, and each part is dried without any water after cleaning. During the cleaning process, automatic cleaning equipment can be used to perform high-strength rotary cleaning on the inner tank 2. For example, high-temperature and high-pressure spray guns are used for cleaning, or special equipment is used for high-power cleaning. It should be noted that when the inner tank 2 is cleaned, the air duct 26 needs to be sprayed with high-pressure water flow from the connecting port into the air duct 26, and then blown with high-pressure air flow after drying.

[0039] In step S2, the device is assembled; including the following steps: Step B1: The refrigeration temperature control device 5 is assembled and fixed in the outer tank 1: first, the refrigeration temperature control device 5 is installed and fixed on the bottom of the lower outer tank 12, and the evaporator copper pipe 51 is installed and fixed on the baffle 121 and arranged in the interlayer between the inner tank 2 and the outer tank 1, and the entire refrigeration temperature control device 5 is connected to form an independent device or system that can cool and control the refrigeration temperature.

[0040] Step B2: The upper outer tank 11 and the inner tank 2 are assembled and fixed: the upper outer tank 11 and the inner tank 2 are connected as a whole at the tank neck through the connecting filler, and different connection methods are used according to different materials. When the tank is made of corrosion-resistant metal, the two can be connected as a whole by welding. The reason for such arrangement is to facilitate the arrangement and placement of the air duct 26. The air duct 26 is connected to the inner tank 2 as a whole by welding, and a connecting port is arranged near the nitrogen cylinder cavity 21 of the air duct 26.

[0041] Step B3: Assembly of inner and outer tank bodies: the assembled upper outer tank body 11 is covered on the lower outer tank body 12, and the inner tank body 2 is inserted into the lower outer tank body 12; two vertical plates are arranged between the two evaporator copper pipes 51 clamped by the inner tank body 2 and the lower outer tank body 12. The two vertical plates are arranged on the inner side walls of the lower outer tank body 12 and the upper outer tank body 11 in advance, and are disconnected at the upper mounting table 111 and the lower mounting table 125 and connected by a plug-in structure. If necessary, two Z-shaped positioning blocks embedded in each other are arranged at the connection to close the inner tank body 2 in the upper outer tank body 11 and the lower outer tank body 12, and the positioning is performed when the embedding is performed. The upper outer tank body 11 and the lower outer tank body 12 are connected as a whole so that the tank wall of the lower outer tank body 12 and the pipe wall of the inner tank body 2 jointly form a filling cavity with the two vertical plates after the inner tank body 2 is inserted into the outer tank body 1 for filling.

[0042] It should be noted that when the inner and outer tank bodies are assembled, one of the filling cavities is used as a reserved cavity for electric wires and control lines when the vertical plates are arranged, and the control lines and electric wires are pre-buried in the cavity and connected with each other during assembly. At the same time, before assembly, a layer of thermal insulation layer is coated on the wall surface of the inner tank body 2 except the outer wall, or a material that has both thermal insulation and supporting functions is selected as the filler when the filler 4 is selected.

[0043] Step B4: injection of filler and fixation of tank body: the bolt hole is used as a filler injection hole, and the filler is injected between the inner and outer tank bodies for clamping and filling. After the filler is injected and fixed and formed, the upper outer tank body 11 and the lower outer tank body 12 are fastened by bolts. The bolt hole, which is used as a filler injection hole, is also used as one of the fastening connection structures for connecting the inner and outer tank bodies. A screw thread or a screw tooth is arranged in the bolt hole, and then the bolt is fastened. At the same time, the bolt is also screwed into the filler for connection.

[0044] Step S3: verification of the assembled tank body and final cleaning, including the following steps: Step C1: electrical connection; the electric wires and control lines of the pressure sensor 29, the electromagnetic air valve 24, and the cold temperature control device are passed through the reserved channel and connected to the first controller, and the high-pressure nitrogen cylinder 22 is placed in the nitrogen cylinder cavity 21 and connected to the electromagnetic air valve 24 and the air duct 26.

[0045] Step C2: manual verification of inflation; the first controller and the pressure sensor 29 at the tank opening are used for manual verification. First, whether the nitrogen gas can be normally blown out from the air hole 27 is checked by controlling the opening and closing of the electromagnetic air valve 24 through the first controller; then whether the nitrogen gas can be normally blown out from the air hole 27 by controlling the pressure of the pressure sensor 29 is checked. If not, the connection equipment and control equipment are checked again for verification.

[0046] Step C3: automatic verification of inflation or sealing verification; verification is performed by installing the tank cover 3, when the tank cover 3 is opened, whether the pressure sensor 29 can normally control the nitrogen gas to be blown out from the air hole 27, when the tank cover 3 is closed, whether the tank can reach the predetermined pressure, if not, check the connection equipment and control equipment and then verify again.

[0047] Step C4: air wall verification; place a high-precision humidity sensor in the tank and outside the tank, open the electromagnetic air valve 24 to form an air wall and overflow gas, change the external humidity, and check whether the humidity in the tank changes, if it changes, check whether the air pressure of the formed air wall reaches the sealing pressure requirement, adjust the pressure and verify again.

[0048] Step C5: refrigeration temperature control verification; the storage temperature of the inner tank body 2 installed and verified in steps C2, C3 and C4 is controlled to verify whether it can normally refrigerate and maintain at the set temperature.

[0049] Step C6: pre-filling cleaning; before filling, the inner tank body 2 is finally cleaned with germanium tetrachloride.

[0050] The application is completed after filling, and after filling is completed, nitrogen gas is filled to the top of the first control nitrogen cylinder 22 and maintained at a certain pressure, and the use is completed. When the tank cover 3 is opened, due to the loosening of the tank cover 3, the internal pressure changes, and at the same time the pressure sensor 29 detects that the tank cover 3 is opened, the first controller controls the electromagnetic air valve 24 to appropriately fill nitrogen gas, and when the tank cover 3 is completely opened, it normally operates, so that the air hole 27 sprays gas flow to form an air wall at the tank opening and overflow gas flow outward, so that external air can not enter the tank. As long as the tank opening 210 is in an open state, the air wall and the outward overflow gas flow exist all the time, even if the product in the tank is sampled or other taken out operation, the external air will not enter the tank, even if the product in the tank is taken out a certain capacity, the empty space will be filled with nitrogen gas released by the nitrogen cylinder 22, the storage environment in the tank is maintained, and the product is prevented from being volatilized and contacted with external moisture.

[0051] By using the method of the application, the storage device is used to avoid the failure of sealing and storage of the device as much as possible, and to ensure that the purity of the high-purity germanium tetrachloride for optical fiber storage is not reduced due to sampling or opening during use.

[0052] Finally, it should be noted that the terms "first" and "second", and the like, are used herein only to distinguish one identification entity from another, and do not require or imply these entities to be in any physical or logical order. Moreover, the terms "comprising", "including", or any other variation thereof, are intended to cover a non-exclusive inclusion, such that processes, methods, articles, or apparatuses that comprise, include, or are otherwise encompassed by a series of elements, do not require that all of the elements be present, only that some, but not necessarily all, of the elements are present to provide the processes, methods, articles, or apparatuses.

[0053] The units described as separate components may or may not be physically separate, and the components displayed as units may or may not be physical units, i.e. may be located in one place, or may be distributed to multiple network units. Part or all of the units can be selected according to actual needs to achieve the purpose of the embodiment.

[0054] The above has described the embodiments of the present application, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments. The selection of the terms used herein is intended to best explain the principles, practical application or improvement of the technology in the market of the embodiments, or to enable other ordinary skilled persons in the art to understand the embodiments disclosed herein.

Claims

1. A high-purity germanium tetrachloride storage device for optical fibers, comprising a cooling and temperature control device (5), characterized in that, Also includes: The outer tank (1) is composed of two parts, namely an upper outer tank (11) and a lower outer tank (12), the upper outer tank (11) and the lower outer tank (12) being detachably and securely connected; the bottom of the lower outer tank (12) is constructed with a baffle (121) to divide it into a bottom refrigeration temperature control device cavity (122); and An inner tank (2) is provided with a nitrogen cylinder cavity (21) on its outside, and a nitrogen cylinder (22) is provided inside the nitrogen cylinder cavity (21); a can opening (210) is constructed on the top of the inner tank (2); a gas passage (26) is provided on the outer top of the inner tank (2) near the can opening (210), and a gas hole (27) is constructed on the inner tank (2) below the can opening (210) to connect the gas passage (26) with the interior of the inner tank (2), and the gas passage (26) is connected to the nitrogen cylinder (22) inside the nitrogen cylinder cavity (21) through a gas pipe (25); and The can lid (3) is equipped with a pump (31). The inlet of the pump (31) is connected to an inner tube (32) that is inserted into the inner tank (2). The outlet of the pump (31) is connected to an outer tube (33). A valve (34) is installed on the outer tube (33). The inner tank (2) is placed inside the outer tank (1) to form a sandwich, the refrigeration temperature control device (5) is placed inside the refrigeration temperature control device cavity (122), and the evaporator copper tube (51) of the refrigeration temperature control device (5) is placed inside the sandwich.

2. The high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The baffle (121) is an annular plate with a hollow center and mounting holes (123) for placing the copper tube (51) of the evaporator.

3. The high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The interlayer is filled with a filler (4).

4. A high-purity germanium tetrachloride storage device for optical fibers according to claim 3, characterized in that: The filler (4) is a heat insulation and structural support filler.

5. A high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The outer tank (11) and the inner tank (2) are connected as a whole at the neck by a connecting filler.

6. A high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The air passage (26) is arranged around the shoulder of the tank, and the air holes (27) are multiple and arranged obliquely upward.

7. A high-purity germanium tetrachloride storage device for optical fibers according to claim 6, characterized in that: The inclination angle of the pore (27) is 5 to 15 degrees.

8. A high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: A pressure sensor (29) is embedded in the top of the can opening (210), and an electromagnetic valve (24) is provided on the air pipe (25). The pressure sensor (29) and the electromagnetic valve (24) are connected to a first controller that integrates display and control. The first controller is embedded in the outer can body (1).

9. A high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The connection between the upper outer tank (11) and the lower outer tank (12) is provided with an upper mounting platform (111) and a lower mounting platform (125) that fit together. After the upper mounting platform (111) and the lower mounting platform (125) fit together, they are fastened with screws.

10. A high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: The bottom of the can lid is equipped with a corrosion-resistant sealing ring (6).