Tubular fluorination reactor
The innovative design of the tubular fluorination reactor solves the problems of high energy consumption, poor heat dissipation, low reaction efficiency, and heavy maintenance of traditional reactors, achieving efficient heat transfer and material utilization, and improving production capacity and equipment stability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-12
- Publication Date
- 2026-03-13
AI Technical Summary
Existing methods for synthesizing metal fluorides and their reactor designs suffer from problems such as high energy consumption, poor heat dissipation, low reaction efficiency, significant material loss, and heavy maintenance workload.
The tubular fluorination reactor is designed with an inverted conical feeding hopper, a conical solid waste collection hopper, a closed-loop circulation system formed by wound copper tubes and a circulating pump. Combined with a finned structure, it achieves efficient heat transfer and material pretreatment, increases the contact area, and is equipped with a sieve plate to filter solid waste.
It improves heat dissipation efficiency and fluorinator utilization, reduces material loss, lowers energy consumption, extends equipment life, and increases production capacity and reaction efficiency.
Smart Images
Figure CN223988452U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of inorganic fluorination technology, and more specifically, to a tubular fluorination reactor. Background Technology
[0002] In the semiconductor industry, tungsten hexafluoride (WF6), ruthenium hexafluoride (RuF6), molybdenum hexafluoride (MoF6), and rhenium hexafluoride (ReF6) are key raw materials widely used in the chemical vapor deposition (CVD) process of metallic tungsten, ruthenium, molybdenum, and rhenium. These fluorides play a crucial role in the manufacture of high-performance integrated circuits due to their unique chemical and physical properties.
[0003] Currently, there are two main methods for synthesizing the four metal fluorides mentioned above. The first method involves reacting metal powder with high-purity nitrogen trifluoride (NF3) to generate the corresponding metal fluorides, which are then purified to obtain tungsten hexafluoride, ruthenium hexafluoride, molybdenum hexafluoride, and rhenium hexafluoride, suitable for integrated circuit manufacturing. The second method involves reacting metal powder directly with fluorine gas (F2), which can also produce the desired metal fluorides.
[0004] However, both synthesis methods currently employ horizontal reactors. These reactors are typically equipped with external heating elements to provide the necessary temperature conditions for the reaction. During operation, the metal powder is added to half the reactor cavity and preheated by external heating devices to remove water. This step is not only energy-intensive but also inefficient.
[0005] After dehydration, the reactor is further heated to the reaction temperature, and then a fluorinating agent (either nitrogen trifluoride or fluorine gas) is introduced to carry out the reaction. Because the reaction releases a large amount of heat, traditional air cooling methods are ineffective, often requiring strict control of the fluorinating agent feed rate to avoid overheating and safety hazards. This limitation directly affects the reactor's capacity and efficiency.
[0006] Furthermore, existing reactor designs suffer from low reaction efficiency. Since the reaction occurs only at the interface between the metal powder and the fluorinating agent, the contact area gradually decreases as the reaction proceeds, leading to a decrease in the reaction rate, a reduction in the conversion rate of the fluorinating agent, and an increase in material loss.
[0007] More seriously, the fluorination reaction of metal powder is extremely sensitive to impurities (such as oxygen and water), which can form metal fluoride powder deposits at the bottom of the reactor. This not only affects the normal operation of the reactor but also increases the workload of periodically disassembling the reactor for cleaning and replacement, further reducing production efficiency.
[0008] In summary, existing methods for synthesizing metal fluorides and their reactor designs suffer from numerous problems, including high energy consumption, poor heat dissipation, low reaction efficiency, significant material loss, and heavy maintenance workload. Utility Model Content
[0009] Based on the above problems, this application proposes a tubular fluorination reactor to solve the technical problems of high energy consumption, poor heat dissipation, low reaction efficiency, serious material loss and large maintenance workload in traditional reactor designs.
[0010] To solve the above-mentioned technical problems, the technical solution adopted by this utility model is as follows:
[0011] A tubular fluorination reactor includes a reactor body, an upper cylindrical feeding chamber at the upper end of the reactor body, and a lower cylindrical solid waste collection chamber at the lower end of the reactor body. A first copper tube is wound around the outside of the reactor body, and a second copper tube is wound around the outside of the upper cylindrical feeding chamber. The first and second copper tubes are connected by a circulation pump. Fins are provided inside the reactor body. A fluorinating agent inlet is provided at the upper part of the reactor body, and a gas outlet is provided at the lower end of the reactor body. A nitrogen inlet is provided at the bottom of the side wall of the upper cylindrical feeding chamber. A vacuum outlet and a solid feed inlet are provided at the upper part of the upper cylindrical feeding chamber. A sieve plate is provided between the reactor body and the lower cylindrical solid waste collection chamber.
[0012] In one specific implementation, a valve is provided between the reactor body and the upper cylindrical feeding hopper, and the reactor body is connected to the lower cylindrical solid waste collection hopper via a flange.
[0013] In one specific implementation scheme, the outlet of the first copper pipe on one side is connected to the inlet of the circulation pump, the inlet of the second copper pipe on one side is connected to the outlet of the circulation pump, and the inlet of the first copper pipe on the other side is connected to the outlet of the second copper pipe on the other side, forming a closed loop of circulation with the first copper pipe, the second copper pipe and the circulation pump.
[0014] In one specific implementation scheme, the upper cylindrical feeding hopper is inverted conical, the lower cylindrical solid waste collection hopper is conical, and the lower cylindrical solid waste collection hopper is provided with a discharge port.
[0015] In one specific implementation, the aperture of the sieve plate is 6-8 mm, and the thickness of the sieve plate is 20-50 mm.
[0016] In one specific feasible implementation, the first copper tube and the second copper tube contain high-temperature heat-conducting oil.
[0017] The positive effects of this utility model are:
[0018] 1. The reactor in this invention is externally wound with copper pipes, and a circulating pump is used to force the heat transfer oil to circulate, transferring the heat released from the fluorinating agent inlet and the main reaction zone at the top of the reactor to the bottom of the reactor. This has two effective effects: firstly, it improves the heat dissipation efficiency of the main reaction zone, protecting the equipment, and also helps to increase the intake of fluorinating agent, thus increasing the production capacity of a single reactor; secondly, it transfers the heat from the main reaction zone to the bottom of the reactor, keeping the bottom of the reactor above the temperature required for the reaction, thereby allowing the unreacted fluorinating agent in the main reaction zone to further fluorinate in the bottom of the reactor, greatly improving the utilization rate of the fluorinating agent.
[0019] 2. This invention is a tubular reactor with the fluorinating agent entering from the top and exiting from the bottom, resulting in a large contact area with the metal material and improving the utilization rate of the fluorinating agent.
[0020] 3. The tubular reactor of the present invention is equipped with a solid waste collection bin at the bottom. Metal fluoride oxide powder that is inevitably generated during the production process is collected in the collection bin and discharged periodically, reducing downtime for maintenance and repair.
[0021] 4. The circulating pump transfers the heat from copper pipe I to copper pipe II, which is wound around the upper feeding hopper. The reaction preheating pretreatment of the metal raw materials removes surface moisture and further reduces energy consumption.
[0022] 5. The reactor is designed with fins inside, which increases heat dissipation and improves the production capacity of a single reactor. Attached Figure Description
[0023] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of this application. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.
[0024] Figure 1 This is a schematic diagram of the structure of this utility model;
[0025] Figure 2 This is a schematic diagram of the structure of this utility model during operation;
[0026] Explanation of reference numerals in the attached figures
[0027] 1. Reactor body; 2. Upper cylinder feeding bin; 3. Lower cylinder solid waste collection bin; 4. First copper pipe; 5. Second copper pipe; 6. Circulation pump; 7. Fins; 8. Gas outlet; 9. Fluoride inlet; 10. Nitrogen inlet; 11. Vacuum outlet; 12. Solid feed port; 13. Sieve plate; 14. Valve; 15. Flange; 16. Drain port. Detailed Implementation
[0028] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.
[0029] Example
[0030] like Figure 1-2 As shown, a tubular fluorination reactor includes a reactor body 1, with an upper cylindrical feeding chamber 2 at the upper end of the reactor body 1. The upper cylindrical feeding chamber 2 is inverted conical in shape. The design of the upper cylindrical feeding chamber 2 inverted conical shape facilitates the addition and premixing of solid raw materials, and at the same time promotes the uniform distribution of raw materials, improves the utilization rate of raw materials and the uniformity of the reaction, and provides favorable conditions for the efficient fluorination reaction.
[0031] The lower end of the reactor body 1 is provided with a lower cylindrical solid waste collection chamber 3, which is conical. The solid waste collection chamber is provided with a discharge port 16, which is also conical, to facilitate the collection and discharge of solid waste, reduce downtime for maintenance and repair, and maintain the cleanliness and efficient operation of the reactor by regularly discharging solid waste, thus extending the service life of the equipment.
[0032] A first copper tube 4 is wound around the outer side of the middle section of the reactor body 1, and a second copper tube 5 is wound around the outer side of the upper cylindrical feeding hopper 2. The first copper tube 4 and the second copper tube 5 are connected by a circulation pump 6. On one side, the outlet of the first copper tube 4 is connected to the inlet of the circulation pump 6, and on the other side, the inlet of the first copper tube 4 is connected to the outlet of the circulation pump 6. The first copper tube 4, the second copper tube 5, and the circulation pump 6 form a closed-loop circulation system. High-temperature heat transfer oil is contained inside the first copper tube 4 and the second copper tube 5. Wound around the outer side of the reactor body 1 and the upper cylindrical feeding hopper 2, the high-temperature heat transfer oil is forcibly circulated by the circulation pump 6, achieving effective heat transfer. On the one hand, this improves the heat dissipation efficiency of the main reaction zone and protects the equipment; on the other hand, it transfers the heat from the main reaction zone to the lower part of the reactor, allowing unreacted fluorinating agent to further fluorinate in the lower part of the reactor, improving the utilization rate of the fluorinating agent. At the same time, the reaction preheating pretreatment of the metal raw materials removes surface moisture and reduces energy consumption.
[0033] The reactor body 1 is equipped with fins 7 inside. The fins 7 are located inside the reactor, which increases the heat dissipation area and improves the heat dissipation effect. By increasing the heat dissipation area, the heat dissipation efficiency of the reactor is improved, and the production capacity of a single reactor is further improved.
[0034] The upper part of the reactor body 1 is provided with a fluorinating agent inlet 9, the lower end of the reactor body 1 is provided with a gas outlet 8, the bottom of the side wall of the upper cylindrical feeding bin 2 is provided with a nitrogen inlet 10, the upper part of the upper cylindrical feeding bin 2 is provided with a vacuum outlet 11 and a solid feeding port 12, and a sieve plate 13 is provided between the reactor body 1 and the solid waste collection bin.
[0035] A valve 14 is provided between the reactor body 1 and the upper cylinder feeding hopper 2, and the reactor body 1 is connected to the lower cylinder solid waste collection hopper 3 by a flange 15.
[0036] The sieve plate 13 has an aperture of 6-8 mm and a thickness of 20-50 mm. The sieve plate 13 is positioned between the reactor body 1 and the solid waste collection chamber, and its suitable aperture and thickness enable effective filtration of solid waste. Through the filtration effect of the sieve plate 13, the smooth discharge of solid waste is ensured, while simultaneously preventing the solid waste from affecting the reactor body 1, thus improving the stability and durability of the equipment.
[0037] Working principle
[0038] The fluorination reaction proceeds as follows:
[0039] Solid raw materials are added through the solid feed port 12 of the upper cylinder feed hopper 2. The feed hopper is designed in an inverted cone shape, which is beneficial for the uniform distribution and premixing of the raw materials. The fluorinating agent enters the reactor through the fluorinating agent inlet 9 at the top of the reactor body 1 and undergoes a fluorination reaction with the solid raw materials. The gas produced by the reaction is discharged through the gas outlet 8 at the bottom of the reactor body 1, completing the reaction process.
[0040] Heat transfer and management:
[0041] The reactor body 1 and the upper cylindrical feeding hopper 2 are respectively wound with a first copper tube 4 and a second copper tube 5, both filled with high-temperature heat transfer oil. A circulating pump 6 extracts the high-temperature heat transfer oil from the first copper tube 4 through a pipeline and pumps it into the second copper tube 5, forming a closed-loop circulation. Inside the reactor body 1, the heat generated by the reaction is transferred to the high-temperature heat transfer oil in the first copper tube 4 via heat conduction. The heated oil is then pumped by the circulating pump 6 to the second copper tube 5 to preheat the raw materials in the upper cylindrical feeding hopper 2, removing surface moisture. Simultaneously, the heat transfer oil in the second copper tube 5 transfers heat to the upper cylindrical feeding hopper 2. The preheated raw materials entering the reactor body 1 can reach the reaction temperature more quickly, improving reaction efficiency. This heat transfer method not only improves the heat dissipation efficiency of the main reaction zone and protects the equipment, but also increases the utilization rate of the fluorinating agent and the reactor's production capacity.
[0042] Raw material pretreatment:
[0043] The upper cylinder feeding hopper 2 has a nitrogen inlet 10 at the bottom of its side wall, which allows nitrogen to be introduced to inertize the raw materials and prevent them from reacting with oxygen in the air during the feeding process. The upper part of the upper cylinder feeding hopper 2 has a vacuum outlet 11, which allows the feeding hopper to be evacuated before feeding to further ensure the purity of the reaction environment.
[0044] Collection and treatment of solid waste:
[0045] Solid waste, such as metal fluoride oxide powder, generated during the reaction falls through sieve plate 13 into the solid waste collection bin 3 in the lower cylinder. Sieve plate 13 has a suitable pore size and thickness, effectively filtering the solid waste and preventing it from entering the reactor body 1 and affecting the reaction process. The solid waste collection bin is designed in a conical shape with a drain port 16 at the bottom for convenient periodic discharge and collection of solid waste. Periodic discharge of solid waste maintains the cleanliness and efficient operation of the reactor, extending the equipment's service life.
[0046] Finally, it should be noted that in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.
[0047] The above description of the disclosed embodiments enables those skilled in the art to make or use this application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this application. Therefore, this application is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A tubular fluorination reactor characterized by, The utility model relates to a reactor for fluorination reaction, including reactor body (1), the upper end of reactor body (1) is provided with upper cylinder charging bin (2), the lower end of reactor body (1) is provided with lower cylinder solid waste collection bin (3), the outside of reactor body (1) is wound with first copper pipe (4), the outside of upper cylinder charging bin (2) is wound with second copper pipe (5), and the first copper pipe (4) and the second copper pipe (5) are communicated by circulation pump (6), the inside of reactor body (1) is provided with fin (7), the upper portion of reactor body (1) is provided with fluorination agent import (9), and the lower end of reactor body (1) is provided with gas outlet (8), the bottom of the side wall of upper cylinder charging bin (2) is provided with nitrogen import (10), the upper portion of upper cylinder charging bin (2) is provided with vacuum export (11) and solid feeding port (12), and the reactor body (1) is provided with screen plate (13) between lower cylinder solid waste collection bin (3).
2. A tubular fluorination reactor according to claim 1, wherein Valve (14) is arranged between reactor body (1) and upper cylinder charging bin (2), and reactor body (1) is connected with lower cylinder solid waste collection bin (3) through flange (15).
3. The tubular fluorination reactor according to claim 1, wherein The outlet of one side first copper pipe (4) is communicated with the import of circulation pump (6), the import of one side second copper pipe (5) is communicated with the outlet of circulation pump (6), and the import of the other side first copper pipe (4) is communicated with the outlet of the other side second copper pipe (5), and first copper pipe (4), second copper pipe (5) and circulation pump (6) form a closed loop.
4. The tubular fluorination reactor of claim 1, wherein, The upper cylinder charging bin (2) is inverted conical, the solid waste collection bin is conical, and the bottom of the lower cylinder solid waste collection bin (3) is provided with a net discharge port (16).
5. The tubular fluorination reactor according to claim 1, wherein The aperture of the screen plate (13) is 6-8mm, and the thickness of the screen plate (13) is 20-50mm.
6. The tubular fluorination reactor of claim 1, wherein, The first copper pipe (4) and the second copper pipe (5) have high-temperature heat-conducting oil.