Device for preparing germanium tetrafluoride through direct fluorination of fluorine gas and use method
By combining a horizontal fluorination reactor with a motor-driven rotating shaft, the problems of temperature control and purity in the preparation of germanium tetrafluoride were solved, achieving an efficient and safe fluorination process, reducing energy and raw material consumption, and improving product purity.
Patent Information
- Application Number
- CN202511590917.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-03
- Publication Date
- 2026-01-27
AI Technical Summary
In the existing technology for preparing germanium tetrafluoride, the reaction temperature is difficult to control, which can easily lead to explosion. Furthermore, the use of dilution gas and excessive fluorine increases energy consumption and raw material costs. At the same time, batch feeding can easily cause material accumulation and air ingress, reducing product purity.
A horizontal fluorination reactor is used, combined with a motor-driven rotating shaft and lifting plates, to achieve the spreading and aggregation of materials. The use of corrosion-resistant material Monel400 ensures the uniformity and sealing of the reaction. Impurities are removed through a filter to achieve the preparation of high-purity germanium tetrafluoride.
Effective control of reaction temperature avoids the risk of explosion, reduces energy consumption and raw material costs, improves product purity and production efficiency, and simplifies the equipment structure.
Smart Images
Figure CN121402009A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of fluoride preparation technology, specifically to an apparatus and method for directly fluorinating germanium tetrafluoride with fluorine gas. Background Technology
[0002] Germanium tetrafluoride is widely used in the field of semiconductor materials. The direct reaction of germanium with fluorine gas to produce germanium tetrafluoride is a common method for its preparation. However, the reaction is highly exothermic, making it difficult to control the reaction temperature. If the heat cannot be removed in time after the reaction begins, it may lead to an explosion.
[0003] In existing technologies, the reaction rate is mainly controlled by diluting fluorine gas with inert gas or by feeding in batches. Using inert gas to dilute fluorine gas not only increases energy consumption as the dilution gas enters the subsequent condensation and collection system along with germanium tetrafluoride gas, but also increases raw material costs due to the discharge of excess fluorine gas. To avoid resource waste caused by the discharge of excess fluorine gas, some researchers have proposed using a circulating pump to return excess fluorine gas to the reactor, which not only increases energy consumption but also increases the complexity of the equipment. While batch feeding can better control the reaction rate, material accumulation can easily cause localized overheating, and multiple feedings can allow air to enter the reactor, reducing product purity and increasing the load on the subsequent purification system, which is detrimental to industrial production. Summary of the Invention
[0004] The purpose of this invention is to provide an apparatus and method for the direct fluorination of fluorine to prepare germanium tetrafluoride, which is used for the intermittent fluorination production of high-purity germanium tetrafluoride by gas-solid reaction.
[0005] The technical solution of the present invention is as follows: an apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride, comprising a horizontal fluorination reactor, a storage silo connected in the middle of the horizontal fluorination reactor, and a feeding ball valve installed below the storage silo; a motor connected to the horizontal fluorination reactor via a coupling, the motor driving a rotating shaft to rotate, and a lifting plate on the rotating shaft; a discharge port located directly below the horizontal fluorination reactor; an outlet on one side of the horizontal fluorination reactor, the outlet being connected to a filter, the filter containing a filter element.
[0006] The feed ball valve has an open / close indicator. By opening and closing the feed ball valve, the raw materials in the storage silo are added into the horizontal fluorination reactor.
[0007] The lifting plates connected to the rotating shaft are axially symmetrical with the feed inlet as the center. The lifting plates are tilted at an angle of 30° relative to the rotating shaft. The motor has two modes: forward and reverse. The forward and reverse rotation of the motor correspond to the two modes of material polymerization and material spreading in the fluorination reactor, respectively.
[0008] The storage silo is equipped with male and female flange sealing covers, and the flanges are sealed with PTFE gaskets.
[0009] The horizontal fluorination reactor has rotary seals on both sides, and the rotary seals include flexible graphite packing, gland, and ceramic bearings.
[0010] Temperature and pressure display instruments are connected to the top of the horizontal fluorination reactor.
[0011] The discharge port outlet uses male and female flanges for connection, and PTFE gaskets are used to seal between the flanges.
[0012] The horizontal fluorination reactor is fixed at its lower sides by grounding plates; the motor is fixed by a motor bracket; the rotating shaft of the horizontal fluorination reactor and the rotating shaft of the motor are on the same horizontal line.
[0013] The feeding ball valve, storage silo, filter, and discharge port are made of stainless steel S31603; the rotating shaft, lifting plate, pressure cap, and horizontal fluorination reactor are made of Monel400.
[0014] A method for using an apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride includes the following steps:
[0015] S1: Open the feeding ball valve to add germanium powder from the storage silo into the horizontal fluorination reactor, then close the feeding ball valve; the motor drives the rotating shaft to reverse, thereby dispersing and spreading the germanium powder.
[0016] S2: Fluorine gas is introduced into the horizontal fluorination reactor through the inlet and reacts with germanium powder;
[0017] S3: The gaseous germanium tetrafluoride generated by the reaction is discharged through the outlet and filtered through a filter;
[0018] S4: Open the discharge port, the motor drives the rotating shaft to rotate forward, causing the powder to gather and discharge unreacted germanium powder and impurities from the discharge port.
[0019] The significant advantage of this invention is that, compared with the prior art, this application achieves the following:
[0020] (1) The horizontal fluorination reactor and its key components are made of Monel400 material, which makes the fluorination device corrosion resistant and solves the problems of leakage and insufficient product purity caused by corrosion of equipment by fluoride or raw materials during the preparation of fluoride.
[0021] (2) The rotating shaft is driven by a motor to spread the material to both sides after it is added, which avoids the problem of insufficient fluorination caused by material agglomeration or uneven spreading after adding the material, and improves the reaction rate of the fluorination process.
[0022] (3) By driving the motor to rotate the axial material in the middle, the impurities and solid materials in the fluorination reactor are removed, thus avoiding the long-term accumulation of materials in the fluorination reactor, which would cause the materials to deteriorate or have too many impurities, affecting the purity of the fluorinated products. Attached Figure Description
[0023] Figure 1 This is a schematic diagram of a germanium tetrafluoride fluorination device.
[0024] The markings in the diagram are as follows: 1-Motor, 2-Coupling, 3-Gland, 4-Bearing, 5-Graphite packing, 6-Lifting plate, 7-Air inlet, 8-Ground plate, 9-Storage silo, 10-Feeding ball valve, 11-Discharge port, 12-Filter, 13-Filter element, 14-Air outlet, 15-Horizontal fluorination reactor, 16-Rotating shaft. Detailed Implementation
[0025] Many specific details are set forth in the following description to provide a full understanding of this application. However, this application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of this application; therefore, this application is not limited to the specific embodiments disclosed below.
[0026] The terminology used in one or more embodiments of this application is for the purpose of describing particular embodiments only and is not intended to limit the scope of one or more embodiments of this application. The singular forms “a,” “the,” and “the” used in one or more embodiments of this application and in the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise. It should also be understood that the term “and / or” used in one or more embodiments of this application refers to and includes any or all possible combinations of one or more associated listed items.
[0027] It should be understood that although the terms first, second, etc., may be used to describe various information in one or more embodiments of this application, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another. For example, first may also be referred to as second without departing from the scope of one or more embodiments of this application, and similarly, second may also be referred to as first.
[0028] The specific technical content of the present invention will now be described with reference to the accompanying drawings;
[0029] An apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride includes a horizontal fluorination reactor 15, a storage silo 9 connected to the middle of the horizontal fluorination reactor 15, and a feeding ball valve 10 installed below the storage silo 9. The feeding ball valve 10 has a valve open / close indicator. By opening and closing the feeding ball valve 10, the raw material in the storage silo 9 can be added into the horizontal fluorination reactor 15.
[0030] Preferably, the storage silo 9 is equipped with a male and female flange sealing cover, and the flanges are sealed with PTFE gaskets; the lower end of the feeding ball valve 10 is connected to the center of the horizontal fluorination reactor 15.
[0031] Motor 1 is connected to horizontal fluorination reactor 15 via coupling 2. Motor 1 drives rotating shaft 16 to rotate, and rotating shaft 16 is equipped with lifting plate 6.
[0032] Specifically, the motor 1 can be adjusted to two modes: forward and reverse rotation. The lifting plate 6 connected to the rotating shaft 16 is axially symmetrical about the feed inlet. The lifting plate 6 is tilted at an angle of 30° relative to the rotating shaft 16. The forward and reverse rotation of the motor 1 correspond to the two modes of material polymerization and material spreading in the fluorination reactor 15, respectively. After the feeding is completed, the motor 1 reverses to spread the material, and during the reaction, the motor 1 rotates forward to polymerize the material.
[0033] The horizontal fluorination reactor 15 is connected to the pressure cap 3 at both ends, and the motor 1 passes through the pressure cap 3. The pressure cap 3 seals the left and right ends of the horizontal fluorination reactor 15.
[0034] Specifically, temperature and pressure display instruments are connected to the top of the horizontal fluorination reactor 15;
[0035] The discharge port 11 is located directly below the horizontal fluorination reactor 15. The outlet of the discharge port 11 is connected by a male and female flange, and a PTFE gasket is used to seal between the flanges.
[0036] The horizontal fluorination reactor 15 has an outlet 14 on one side above the filter 12, which is connected to the filter 12. The filter 12 contains a filter element 13, and the filter element 13 has a flange sealing cover on top.
[0037] Specifically, the horizontal fluorination reactor 15 is fixed on both sides below by grounding plates 8; the motor 1 is fixed by a motor bracket; the rotating shaft 16 of the horizontal fluorination reactor 15 and the rotating shaft of the motor 1 are on the same horizontal line.
[0038] Furthermore, the feeding ball valve 10, storage silo 9, filter cylinder 12, and discharge port 11 are made of stainless steel S31603; the rotating shaft 16, lifting plate 6, pressure cap 3, and horizontal fluorination reactor cylinder 15 are made of Monel 400; and the filter element 13 is made of Monel 400.
[0039] Furthermore, both sides of the horizontal fluorination reactor 15 are rotary seals. The rotary seals include flexible graphite packing 5, pressure cap 3, ceramic bearing 4, sealing cap, intermediate cap, baffle cap, and O-ring. The orderly assembly of the sealing components ensures the sealing performance of the fluorination process.
[0040] In specific work:
[0041] S1: Open the feeding ball valve 10 to add germanium powder from the storage bin 9 into the horizontal fluorination reactor 15, and then close the feeding ball valve 10; the motor 1 drives the rotating shaft 16 to reverse, thereby dispersing and spreading the germanium powder.
[0042] S2: Fluorine gas is introduced into the horizontal fluorination reactor 15 through the inlet 7 and reacts with germanium powder;
[0043] S3: The gas germanium tetrafluoride generated by the reaction is discharged through the outlet 14 and filtered through the filter 12;
[0044] S4: Open the discharge port 11. The motor 1 drives the rotating shaft 16 to rotate clockwise, causing the powder to gather and discharging unreacted germanium powder and impurities from the discharge port 11.
[0045] Specifically, germanium powder was in excess relative to fluorine gas.
[0046] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
[0047] It should be noted that, for the sake of simplicity, the foregoing method embodiments are all described as a series of actions. However, those skilled in the art should understand that this application is not limited to the described order of actions, as some steps may be performed in other orders or simultaneously according to this application. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are preferred embodiments, and the actions and modules involved are not necessarily essential to this application.
[0048] In the above embodiments, the descriptions of each embodiment have different focuses. For parts not described in detail in a certain embodiment, please refer to the relevant descriptions of other embodiments.
[0049] The preferred embodiments disclosed above are merely illustrative of this application. The optional embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this application. These embodiments are selected and specifically described in this application to better explain the principles and practical applications of this application, thereby enabling those skilled in the art to better understand and utilize this application.
Claims
1. An apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride, characterized in that: The system includes a horizontal fluorination reactor (15), a storage silo (9) connected in the middle of the horizontal fluorination reactor (15), and a feeding ball valve (10) installed below the storage silo (9); a motor (1) is connected to the horizontal fluorination reactor (15) through a coupling (2), the motor (1) drives the rotating shaft (16) to rotate, and the rotating shaft (16) is equipped with a lifting plate (6); the discharge port (11) is located directly below the horizontal fluorination reactor (15); there is an outlet (14) on one side of the horizontal fluorination reactor (15), the outlet (14) is connected to a filter (12), and there is a filter element (13) inside the filter (12).
2. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The feed ball valve (10) has a valve open / close indicator. By opening and closing the feed ball valve (10), the raw material in the storage bin (9) is added into the horizontal fluorination reactor (15).
3. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The lifting plate (6) connected to the rotating shaft (16) is axially symmetrical with the feed inlet as the center. The lifting plate (6) is tilted at an angle of 30° relative to the rotating shaft (16). The motor (1) includes two modes: forward rotation and reverse rotation. The forward rotation and reverse rotation of the motor (1) correspond to the two modes of material aggregation and material spreading in the fluorination reactor (15), respectively.
4. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The storage silo (9) is equipped with a male and female flange sealing cover, and the flanges are sealed with PTFE gaskets.
5. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The horizontal fluorination reactor (15) has rotary seals on both sides, and the rotary seals include flexible graphite packing (5), gland (3), and ceramic bearing (4).
6. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: Temperature and pressure display instruments are connected to the top of the horizontal fluorination reactor (15).
7. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The discharge port (11) uses male and female flanges for connection, and PTFE gaskets are used to seal between the flanges.
8. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 1, characterized in that: The horizontal fluorination reactor (15) is fixed on both sides below by grounding plates (8); the motor (1) is fixed by a motor bracket; the rotating shaft (16) of the horizontal fluorination reactor (15) and the rotating shaft of the motor (1) are on the same horizontal line.
9. The apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride according to claim 5, characterized in that: The feeding ball valve (10), storage silo (9), filter (12), and discharge port (11) are made of stainless steel S31603; the rotating shaft (16), lifting plate (6), pressure cap (3), and horizontal fluorination reactor (15) are made of Monel400.
10. A method of using an apparatus for the direct fluorination of fluorine to prepare germanium tetrafluoride, characterized in that: Includes the following steps: S1: Open the feeding ball valve (10) and add germanium powder from the storage bin (9) into the horizontal fluorination reactor (15), then close the feeding ball valve (10); the motor (1) drives the rotating shaft (16) to reverse, thereby dispersing and spreading the germanium powder. S2: Fluorine gas is introduced into the horizontal fluorination reactor (15) through the inlet (7) and reacts with germanium powder; S3: The gas germanium tetrafluoride generated by the reaction is discharged through the outlet (14) and filtered through the filter (12); S4: Open the discharge port (11), the motor (1) drives the rotating shaft (16) to rotate in the forward direction, causing the powder to gather and discharge the unreacted germanium powder and impurities from the discharge port (11).