An apparatus for preparing antimony pentafluoride

Abstract

The utility model discloses a preparation device of antimony pentafluoride, which comprises: an HF absorption tower, a drying tower, a reactor, a filter, a condensing collector and a tail gas absorption tower connected in sequence through pipelines, an air inlet of the HF absorption tower is connected with a nitrogen source and a fluorine-nitrogen source, and an air outlet of the HF absorption tower is connected with a lower end inlet of the drying tower; the reactor is provided with an antimony particle feeding port and is internally provided with a spiral stirring rod extending along an axial direction, and one end of the spiral stirring rod is connected with a motor located outside the reactor. The spiral stirring rod can make the fluorine-nitrogen gas fully contact with the antimony particles, which is conducive to improving the reaction efficiency. The contact time of the antimony pentafluoride generated in the reactor with the reactor is reduced, thereby reducing the risk of corrosion of the reactor under high temperature and the introduction of metal fluoride impurities caused by the contact with the antimony pentafluoride, reducing the difficulty of later purification, and being conducive to realizing efficient, high-purity and safe industrial production.

Description

Technical Field

[0001] This utility model belongs to the field of antimony pentafluoride preparation, and specifically relates to an apparatus for preparing antimony pentafluoride. Background Technology

[0002] Antimony pentafluoride (SbF5), as a highly important inorganic fluoride, plays an irreplaceable core role in the fields of chemical engineering, materials science, and energy. Its applications are wide-ranging and significant for the development of related industries: In superacid systems, it can be mixed with fluorosulfonic acid (HSO3F) or hydrofluoric acid (HF) to form the well-known "magic acid," whose acidity far exceeds that of 100% sulfuric acid. This "magic acid" can even protonate the most stable hydrocarbons, making it crucial in petroleum catalysis, organic synthesis, and basic chemical research. As a strong fluorinating agent, it can effectively replace halogens such as chlorine and bromine in compounds with fluorine atoms, making it a key raw material for the synthesis of fluorinated organic compounds and fluorinated materials. In the field of catalysis, its highly efficient Lewis acid properties make it an important catalyst for reactions such as alkylation, acylation, and polymerization. Furthermore, it is also used in the electronics industry, particularly in the manufacturing processes of semiconductors and liquid crystal displays.

[0003] Currently, industrial-scale and laboratory-scale production of antimony pentafluoride typically employs the direct fluorination method, which involves reacting metallic antimony (Sb) or antimony trichloride (SbCl3) with fluorine gas (F2) or anhydrous hydrogen fluoride (HF). However, antimony pentafluoride is extremely corrosive, reacting with most metals, glass, ceramics, and even quartz at high temperatures. Prolonged exposure to high temperatures and fluorine gas still results in severe corrosion, shortening equipment lifespan and necessitating frequent replacement of critical components such as reaction vessels, pipes, and valves, thus increasing production costs. Furthermore, the metallic fluoride impurities produced by corrosion can contaminate the product, increasing its purity and causing product contamination, thus affecting its application in high-tech fields. Summary of the Invention

[0004] In view of the aforementioned defects in existing antimony pentafluoride preparation apparatus, the purpose of this utility model is to propose an antimony pentafluoride preparation apparatus.

[0005] To achieve the aforementioned objectives, the technical solution adopted by this utility model is as follows: an HF absorption tower, a drying tower, a reactor, a filter, a condenser collector, and a tail gas absorption tower are connected in series via pipelines. The inlet of the HF absorption tower is connected to a nitrogen source and a fluorine-nitrogen source, and its outlet is connected to the lower inlet of the drying tower. The reactor is equipped with an antimony particle feed inlet and an axially extending spiral stirring rod is installed inside. One end of the spiral stirring rod is connected to a motor outside the reactor.

[0006] Furthermore, an axially extending electric heating jacket is installed on the outer wall of the reactor.

[0007] Furthermore, the condenser includes a primary condenser and a secondary condenser, and heating devices are installed on the outer walls of the pipes between the reactor and the primary condenser, as well as on the outer walls of the filter.

[0008] Furthermore, the pipeline heating device is a heating belt, which is equipped with insulation cotton and a temperature probe.

[0009] Furthermore, a jacket is installed on the outer wall of the condenser cylinder, and the jacket is equipped with a refrigerant inlet and a refrigerant outlet.

[0010] Furthermore, the antimony particle feed inlet is equipped with a flange structure.

[0011] Furthermore, the volume fraction of fluorine in the fluorine-nitrogen gas source is 10% to 20%.

[0012] Furthermore, the antimony particles have a particle size of 1~3mm.

[0013] The aforementioned apparatus for preparing antimony pentafluoride can achieve the following beneficial effects: (1) Setting up a spiral stirring rod can make the fluorine and nitrogen gas come into full contact with the antimony particles, which is beneficial to improving the reaction efficiency; (2) The reduced contact time between the antimony pentafluoride produced in the reactor and the reactor reduces the risk of corrosion of the reactor at high temperature and also avoids the risk of introducing impurities due to reactor corrosion, reducing the difficulty of subsequent purification and facilitating efficient, high-purity and safe industrial production.

[0014] The above description is merely an overview of the technical solution of this utility model. In order to better understand the technical means of this utility model and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this utility model more obvious and understandable, preferred embodiments are given below, and detailed descriptions are provided in conjunction with the accompanying drawings. Attached Figure Description

[0015] Figure 1 This is a connection diagram of an apparatus for preparing antimony pentafluoride according to the present invention; Figure 2 yes Figure 1 A schematic diagram of the reactor structure.

[0016] Reference numerals: A: HF absorption tower; B: drying tower; C: reactor; D: filter; E: primary condenser; F: secondary condenser; G: pipeline heating device; H: refrigerant outlet of primary condenser; I: refrigerant outlet of secondary condenser; J: tail gas absorption tower; M: refrigerant inlet of primary condenser; N: refrigerant inlet of secondary condenser; 1: reactor inlet; 2: antimony particle inlet; 3: electric heating jacket; 4: reactor outlet; 5: spiral stirring rod; 6: motor; 7: reactor support. Detailed Implementation

[0017] The features and exemplary embodiments of various aspects of this utility model will now be described in detail. Numerous specific details are set forth in the following detailed description to provide a comprehensive understanding of this utility model. However, it will be apparent to those skilled in the art that this utility model can be practiced without requiring some of these specific details. The following description of embodiments is merely intended to provide a better understanding of this utility model by illustrating examples of it. In the accompanying drawings and the following description, at least some well-known structures and techniques are not shown to avoid unnecessarily obscuring the utility model; and, for clarity, the dimensions of some structures may be exaggerated. The features, structures, or characteristics described below may be combined in any suitable manner in one or more embodiments; furthermore, the terms “first or I,” “second or II,” “third or III,” etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0018] The directional terms used in the following description refer to the directions shown in the figures and are not intended to limit the specific structure of this utility model. It should also be noted in the description of this utility model that, unless otherwise explicitly specified and limited, the terms "set," "install," and "connect" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0019] Please see Figure 1 and Figure 2 This utility model discloses an apparatus for preparing antimony pentafluoride, comprising: an HF absorption tower A, a drying tower B, a reactor C, a filter D, a condenser collector, and a tail gas absorption tower J connected in series via pipelines. The inlet of the HF absorption tower is connected to a nitrogen source and a fluorine-nitrogen source, and its outlet is connected to the lower inlet of the drying tower. The reactor is provided with an antimony particle inlet 2 and an axially extending spiral stirring rod 5 is provided inside it. One end of the spiral stirring rod is connected to a motor 6 located outside the reactor.

[0020] Specifically, fluorine-nitrogen gas and nitrogen gas are introduced into the HF absorption tower. After passing through the drying tower, they enter the reactor through reactor inlet 1 to react with antimony particles. The reaction between fluorine-nitrogen gas and antimony particles is mild and allows for better control of the reaction temperature. Furthermore, the antimony particles have a particle size of 1-3 mm, and the volume fraction of fluorine in the fluorine-nitrogen gas source is 10%-20%. The axially extending spiral stirring rod ensures sufficient contact between the fluorine-nitrogen gas and the antimony particles, which is beneficial for improving reaction efficiency. This reduces the contact time between the antimony pentafluoride produced in the reactor and the reactor, thereby reducing the risk of corrosion of the reactor at high temperatures and lowering costs. Furthermore, reactor supports 7 are installed at both ends of the reactor to support the reactor C. Moreover, the reactor is made of Monel material, and the spiral stirring rod is made of Hastelloy alloy, which enhances the corrosion resistance of the reactor and the spiral stirring rod.

[0021] Please see Figure 2 In another embodiment of this utility model, an axially extending electric heating jacket 3 is provided on the outer wall of the reactor.

[0022] Specifically, the axially extending electric heating jacket ensures stable temperature throughout the reactor. Furthermore, the reactor temperature is 220~240℃ and the pressure is 0.1~0.2Mpa.

[0023] Please see Figure 1 , Figure 2 In another embodiment of the present invention, the condenser collector includes a primary condenser collector E and a secondary condenser collector F. A filter is provided on the pipe between the reactor and the primary condenser collector. A pipe heating device G is provided on the outer wall of the pipe between the reactor and the primary condenser collector and on the outer wall of the filter.

[0024] Specifically, after the reaction is completed, the gas produced by the reaction enters the pipeline through the gas outlet 4 of the reactor. The pipeline heating device heats the pipeline between the filter D and the primary condenser E to 150~180℃. The gas produced by the reaction passes through the filter, the primary condenser, and the secondary condenser in sequence for filtration and purification. The product is collected in the primary condenser and the secondary condenser. The remaining non-condensable gas is discharged after passing through the tail gas absorption tower J.

[0025] Please see Figure 1 In another embodiment of this utility model, the pipeline heating device is a heating belt, and the heating belt is equipped with insulation cotton and a temperature probe.

[0026] Specifically, installing insulation cotton on the outside of the heating belt can reduce heat loss and improve insulation performance, while installing a temperature probe can better control the temperature of the heating belt.

[0027] Please see Figure 1In another embodiment of this utility model, a jacket is provided on the outer wall of the cylinder of the condenser collector, and a refrigerant inlet and a refrigerant outlet are provided on the jacket.

[0028] Specifically, the jacket of the first-stage condenser has a refrigerant inlet M at the bottom and a refrigerant outlet H at the top; the jacket of the second-stage condenser has a refrigerant inlet N at the bottom and a refrigerant outlet I at the top.

[0029] Please see Figure 2 In another embodiment of this utility model, the antimony particle inlet is provided with a flange structure.

[0030] Specifically, the antimony particle feed inlet is equipped with a flange structure and a sealing gasket adapted to the flange structure, so as to achieve better sealing at the feed inlet connection and prevent gas leakage inside the reactor.

[0031] The workflow of the apparatus for preparing antimony pentafluoride according to this invention is as follows: First, the cylinder of reactor C is cleaned and dried. Then, antimony particles are added into the reactor through the antimony particle inlet 2. A pressure test is performed. If the pressure fluctuates within 1 kPa within 1 hour, it is considered to have good airtightness. After that, the reactor is evacuated and purged. The temperature of the electric heating jacket 3 is adjusted to bring the temperature in the reactor to 100~120℃ and maintained for 2~4 hours. Then, the antimony particles and the reactor are dried and purged three times with nitrogen. Fluorine nitrogen gas is introduced into the reactor to make the reactor react under the conditions of 220~240℃ and 0.1~0.2 MPa. The reaction ends when the reaction time meets the process requirements and the reactor pressure remains stable. After the reaction, the pipeline between filter G and primary condenser E is heated to 150~180℃ using a pipeline heating device. The gas produced by the reaction is purified by passing through the filter, primary condenser, and secondary condenser in sequence. The product is collected in the primary and secondary condensers, and the remaining non-condensable gases are discharged after passing through the tail gas absorption tower.

[0032] In other embodiments of this utility model, the pipeline heating device may adopt other types of existing heating structures, such as electric heating jackets, heat medium jackets, etc.

[0033] The above description is merely a preferred embodiment of this utility model. Any simple modifications, equivalent changes, and alterations made by those skilled in the art to the above embodiments based on the technical essence of this utility model without departing from the scope of the technical solution of this utility model shall still fall within the scope of the technical solution of this utility model.

Claims

1. An apparatus for preparing antimony pentafluoride, characterized in that, include: The HF absorption tower (A), drying tower (B), reactor (C), filter (D), condenser collector, and tail gas absorption tower (J) are connected in series by pipelines. The inlet of the HF absorption tower is connected to the nitrogen source and the fluorine-nitrogen source, and its outlet is connected to the lower inlet of the drying tower. The reactor is equipped with an antimony particle feed inlet (2) and an axially extending spiral stirring rod (5) is installed inside it. One end of the spiral stirring rod is connected to a motor (6) located outside the reactor.

2. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, An axially extending electric heating jacket (3) is installed on the outer wall of the reactor.

3. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, The condenser includes a primary condenser (E) and a secondary condenser (F). Pipe heating devices (G) are installed on the outer walls of the pipes between the reactor and the primary condenser, as well as on the outer walls of the filter.

4. The apparatus for preparing antimony pentafluoride according to claim 3, characterized in that, The pipeline heating device is a heating belt, which is equipped with insulation cotton and a temperature probe.

5. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, The outer wall of the condenser is fitted with a jacket, and each jacket has a refrigerant inlet and a refrigerant outlet.

6. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, The antimony particle feed inlet is equipped with a flange structure.

7. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, The volume fraction of fluorine in the fluorine-nitrogen gas source is 10%~20%.

8. The apparatus for preparing antimony pentafluoride according to claim 1, characterized in that, The particle size of the antimony particles is 1~3mm.

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