Large rectifying tower for purifying germanium tetrachloride

Abstract

The large rectifying tower comprises a tower kettle, a tower rod and a tower head which are sequentially connected from bottom to top, the top of the tower kettle is provided with a connector connected with the tower rod, the bottom of the tower kettle is provided with a liquid outlet, and the tower head is provided with an exhaust port and a product outlet. The tower kettle is an enamel kettle which has the capacity of 1000L and is provided with a heating temperature control device, and a feeding hole and a temperature sensor A are arranged at the top of the tower kettle; the tower pole is formed by connecting a plurality of temperature compensators in series; and a temperature sensor B is mounted at the bottom of the tower head. According to the utility model, the purification space is enlarged, the rectifying tower is enlarged, meanwhile, the large-scale and continuous production of germanium tetrachloride is realized by adopting the large-scale tower kettle capable of accurately controlling the heating temperature, and the tower pole is replaced by the temperature compensator consisting of the steel lining polytetrafluoroethylene and the polytetrafluoroethylene sieve plate, so that the temperature change in the tower pole is stabilized after the tower pole is heightened.

Description

Technical Field

[0001] This utility model patent belongs to the technical field of germanium tetrachloride purification equipment, and specifically relates to a large distillation tower used for purifying germanium tetrachloride. Background Art

[0002] High-purity germanium tetrachloride is an important raw material for the production of high-purity germanium dioxide, high-purity germanium single crystals, and optical fiber cables. Ultra-high-purity germanium tetrachloride plays a crucial role in improving the purity and grade of germanium dioxide, zone-melting germanium, and germanium single crystals. During the production of germanium tetrachloride, it undergoes distillation and purification.

[0003] Currently, quartz distillation towers are commonly used for the distillation and purification of germanium tetrachloride. For example, Chinese Patent (CN101269836A) discloses a distillation tower for removing hydrogen-containing impurities from germanium tetrachloride. However, due to the limited material properties, quartz distillation towers are difficult to operate continuously and on a large scale. Therefore, their purification efficiency is low. However, if the above device is to be scaled up, the following technical problems arise:

[0004] 1. Because the temperature control accuracy of germanium tetrachloride distillation needs to be within ±0.5℃, and after the tower is raised to a certain level, the temperature difference between the upper and lower parts of the tower will increase, affecting the purification efficiency;

[0005] 2. At the same time, during the distillation process of germanium tetrachloride, some non-volatile substances will rise with the steam, affecting the purity;

[0006] 3. Because the tower rod is too long, the temperature detection port in the tower kettle cannot monitor the temperature changes in the tower head. In this way, it is difficult to deal with the tower head failure in time.

[0007] Therefore, this paper proposes a large distillation tower for the purification of germanium tetrachloride. Utility Model Content

[0008] In order to solve the above problems, the utility model provides a large-scale distillation tower with high automation degree and high purification efficiency for purifying germanium tetrachloride.

[0009] In order to achieve the above technical effects, the utility model is implemented through the following technical solutions: a large distillation tower for purifying germanium tetrachloride, comprising a tower kettle, a tower rod, and a tower head, and the three are connected in sequence from bottom to top, the top of the tower kettle is provided with an interface connected to the tower rod, the bottom is provided with a liquid outlet, the tower head is provided with an exhaust port and a product outlet, the tower kettle adopts an enamel kettle with a capacity of 1000L and equipped with a heating and temperature control device, the top of the tower kettle is provided with a feed port and a temperature sensor A; the tower rod is composed of several temperature compensators connected in series; and the bottom of the tower head is installed with a temperature sensor B.

[0010] Preferably, the heating and temperature control device also includes a far-infrared electric heating sleeve, an insulating shell, a temperature sensor C, and a control cabinet. The far-infrared electric heating sleeve is mounted on the outside of the enamel kettle, and an insulating shell is installed on the outside of the far-infrared electric heating sleeve. The control cabinet is installed on the left side of the insulating shell, and the temperature sensor C is installed on the right side of the insulating shell.

[0011] Preferably, the control cabinet is connected to the far-infrared electric heating sleeve, temperature sensor A, temperature sensor B, and temperature sensor C by telecommunication.

[0012] Preferably, the temperature compensator in the tower is made of steel lined with PTFE, and a PTFE sieve plate is installed at the connection between adjacent temperature compensators.

[0013] Preferably, a quartz glass coil for cooling reflux is provided in the tower head.

[0014] The beneficial effects of the utility model are:

[0015] This device expands the purification space and enlarges the distillation tower. At the same time, a large tower kettle with precise control of heating temperature is used to achieve large-scale and continuous production of germanium tetrachloride. The tower rod is replaced by a temperature compensator composed of steel-lined PTFE and PTFE sieve plates, so that the temperature changes inside the tower rod can be stabilized after the tower rod is raised. Among them, when passing through the PTFE sieve plates, some non-volatile substances rising with the steam can be filtered, thereby improving the purification efficiency and the purity of germanium tetrachloride. Finally, the temperature changes at each stage of the production process are detected in real time by temperature sensors on the tower kettle and the tower top. In this way, while ensuring production efficiency, it can also deal with faults in a timely manner. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the following briefly introduces the drawings required for describing the embodiments. Those skilled in the art can also obtain other drawings based on these drawings without making any creative efforts.

[0017] Figure 1 It is a structural diagram of the utility model;

[0018] Figure 2 This is a schematic diagram of the structure of the tower kettle of the utility model;

[0019] Figure 3 Schematic diagram of the cross section of the tower of the utility model;

[0020] Figure 4 It is a structural diagram of the tower head of the utility model;

[0021] In the accompanying drawings, the components represented by the reference numerals are as follows:

[0022] 1. Tower kettle; 2. Tower rod; 3. Tower head; 4. Interface; 5. Liquid outlet; 6. Exhaust port; 7. Product outlet; 8. Feed port; 9. Temperature sensor A; 10. Temperature compensator; 11. Temperature sensor B; 12. Far-infrared electric heating jacket; 13. Insulation shell; 14. Temperature sensor C; 15. Control cabinet; 16. PTFE sieve plate; 17. Quartz glass coil. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making creative work are within the scope of protection of the present invention.

[0024] like Figures 1 to 4 As shown, the prior art in this embodiment has the following problems: The inventors discovered that conventional iron removal methods involve removing iron through physical means such as chemical reactions or distillation before the material is formed into powder, but this inevitably leaves trace amounts of iron impurities in the powder. These trace amounts of iron impurities need to be further removed, but there is currently a lack of a simple, compact device for removing iron impurities from high-purity powders.

[0025] Therefore, the inventor provides a large distillation tower for purifying germanium tetrachloride, including a tower kettle 1, a tower rod 2, and a tower head 3, and the three are connected in sequence from bottom to top. The top of the tower kettle 1 is provided with an interface 4 connected to the tower rod 2, and the bottom is provided with a liquid outlet 5. The tower head 3 is provided with an exhaust port 6 and a product outlet 7. The tower kettle 1 adopts an enamel kettle with a capacity of 1000L and is equipped with a heating and temperature control device. The top of the tower kettle 1 is provided with a feed port 8 and a temperature sensor A9; the tower rod 2 is composed of several temperature compensators 10 connected in series; and the bottom of the tower head 3 is installed with a temperature sensor B11.

[0026] The effect is as follows: the device expands the purification space and enlarges the distillation tower. At the same time, a large tower kettle 1 that can accurately control the heating temperature is used to achieve large-scale and continuous production of germanium tetrachloride. The tower rod 2 is replaced by a temperature compensator 10 composed of a steel-lined polytetrafluoroethylene and a polytetrafluoroethylene sieve plate 16, so that the temperature change in the tower rod 2 is stabilized after the tower rod 2 is raised. Part of the non-volatile substances rising with the steam can be filtered when passing through the polytetrafluoroethylene sieve plate 16, thereby improving the purification efficiency and the purity of the germanium tetrachloride. Finally, the temperature changes at each stage of the production process are detected in real time by temperature sensors on the tower kettle 1 and the tower top. In this way, while ensuring production efficiency, it can also be handled in a timely manner when a fault occurs.

[0027] Furthermore, the heating and temperature control device also includes a far-infrared electric heating sleeve 12, an insulating shell 13, a temperature sensor C14, and a control cabinet 15. The far-infrared electric heating sleeve 12 is mounted on the outside of the enamel kettle, and the outer side of the far-infrared electric heating sleeve 12 is installed with an insulating shell 13. The control cabinet 15 is installed on the left side of the insulating shell 13, and the temperature sensor C14 is installed on the right side of the insulating shell 13. The heating sleeve in this structure is a far-infrared electric heating sleeve 12 with a power of 18KW. Under the insulating effect of the insulating shell 13, the temperature control change is controlled within ±0.1°C through the control cabinet 15 and the temperature sensor C14, thereby ensuring the purification efficiency.

[0028] Furthermore, the control cabinet 15 is electrically connected to the far-infrared electric heating jacket 12, the temperature sensor A9, the temperature sensor B11, and the temperature sensor C14; this structure can automate the purification.

[0029] Furthermore, the temperature compensator 10 in the tower 2 is made of steel lined with PTFE, and a PTFE sieve plate 16 is installed at the connection between adjacent temperature compensators 10; this structure can filter some of the non-volatile substances rising with the steam, thereby improving the purification efficiency and the purity of germanium tetrachloride.

[0030] Furthermore, a quartz glass coil 17 for cooling reflux is provided in the tower head 3 .

[0031] The working principle of the utility model is as follows: when in use, germanium tetrachloride to be purified is added into the tower kettle 1 through the feed port 8, and is heated by the heating temperature control device to make the germanium tetrachloride boil and volatilize. The volatilized germanium tetrachloride rises through the tower tube to reach the tower head 3 at the top of the distillation tower, is condensed by the quartz glass coil 17, is collected and can be discharged from the product outlet 7, and the tail gas can be reintroduced into the tower kettle 1 through the exhaust port 6 for heating and distillation. Among them, the temperature sensor can monitor the operating temperature in the tower kettle 1 and the tower head 3 in real time and promptly feed back to the control cabinet 15, and then the control cabinet 15 adjusts the heating temperature to meet the requirements of the process.

[0032] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the present invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be encompassed within the present invention. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0033] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A large-scale distillation tower for purifying germanium tetrachloride, comprising a tower bottom (1), a tower rod (2), and a tower head (3), which are connected in sequence from bottom to top, wherein the top of the tower bottom (1) is provided with an interface (4) connected to the tower rod (2), the bottom is provided with a liquid outlet (5), and the tower head (3) is provided with an exhaust port (6) and a product outlet (7), characterized in that: The tower kettle (1) is an enamel kettle with a capacity of 1000L and equipped with a heating and temperature control device. The top of the tower kettle (1) is provided with a feed port (8) and a temperature sensor A (9); the tower rod (2) is composed of a plurality of temperature compensators (10) connected in series; and the bottom of the tower head (3) is provided with a temperature sensor B (11).

2. A large-scale distillation tower for purifying germanium tetrachloride according to claim 1, characterized in that: The heating and temperature control device further comprises a far-infrared electric heating sleeve (12), a heat-insulating shell (13), a temperature sensor C (14), and a control cabinet (15). The far-infrared electric heating sleeve (12) is sleeved on the outside of the enamel kettle, the heat-insulating shell (13) is installed on the outside of the far-infrared electric heating sleeve (12), the control cabinet (15) is installed on the left side of the heat-insulating shell (13), and the temperature sensor C (14) is installed on the right side of the heat-insulating shell (13).

3. A large-scale distillation tower for purifying germanium tetrachloride according to claim 2, characterized in that: The control cabinet (15) is connected to the far-infrared electric heating sleeve (12), the temperature sensor A (9), the temperature sensor B (11), and the temperature sensor C (14) via telecommunication.

4. A large-scale distillation tower for purifying germanium tetrachloride according to claim 1, characterized in that: The temperature compensator (10) in the tower (2) is made of steel lined with polytetrafluoroethylene, and a polytetrafluoroethylene sieve plate (16) is installed at the connection between adjacent temperature compensators (10).

5. A large-scale distillation tower for purifying germanium tetrachloride according to claim 1, characterized in that: A quartz glass coil (17) for cooling reflux is provided in the tower head (3).

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