Reaction apparatus for reacting solid material with fluorine

Abstract

A kind of reaction device of solid material and fluorine gas reaction, including reactor, first-stage condensation collector, secondary condensation collector, product collection tank, tail gas adsorption tower;The reactor includes the first cylinder of airtight, gas inlet pipe, feed pipe, stirrer, pipe are all worn in the top of first cylinder, the one end of gas inlet pipe is gas inlet, the other end of gas inlet pipe passes through the top of first cylinder and stretches into to the position close to the bottom in first cylinder, gas disperser is provided on gas inlet pipe, the one end of feed pipe is feed inlet, the import and export of pipe are all set in the outside of first cylinder;The outer wall of first cylinder is equipped with electric heating jacket, the side of first cylinder is equipped with gas outlet, gas outlet is connected with the inlet of first-stage condensation collector, the outlet of first-stage condensation collector is connected with the inlet of secondary condensation collector, the discharge port of secondary condensation collector is connected with the inlet of product collection tank, the outlet of secondary condensation collector is connected with the inlet of tail gas adsorption tower.

Description

Technical Field

[0001] This utility model belongs to the field of chemical engineering technology, and specifically relates to a reaction device for reacting solid materials with fluorine gas. Background Technology

[0002] Traditional solid-material fluorine gas reaction devices often employ static reactors (gas-solid reactions), which suffer from uneven fluorine gas distribution, easily leading to localized over-fluorination or side reactions. Fluorine gas is highly corrosive, easily damaging conventional materials (such as stainless steel), resulting in short device lifespan, product contamination, and a high risk of fluorine leakage. The material's contact with fluorine gas is slow, requiring the upper layer to be consumed before contact with the lower layer, resulting in a long reaction time. Temperature control is difficult; some reactions involve sudden releases of large amounts of heat, leading to overheating and product decomposition. The continuous introduction of fluorine and nitrogen gas into the solid powder poses a risk of it being carried away by the gas, causing blockages in subsequent pipelines or valves and increasing maintenance costs. Summary of the Invention

[0003] In order to overcome the shortcomings of the existing technology, this utility model proposes a reaction device for reacting solid materials with fluorine gas.

[0004] The purpose of this utility model is achieved through the following technical solution: a reaction device for reacting solid materials with fluorine gas, comprising a reactor, a primary condenser, a secondary condenser, a product collection tank, and a tail gas adsorption tower; the reactor comprises a sealed first cylinder, with an inlet pipe, a feed pipe, a stirrer, and a coil all passing through the top of the first cylinder. One end of the inlet pipe located outside the first cylinder is the inlet, and the other end of the inlet pipe extends through the top of the first cylinder to a position near the bottom of the first cylinder. A gas disperser is provided at the end of the inlet pipe near the bottom of the first cylinder. The feed pipe located outside the first cylinder is the feed inlet. The inlet and outlet of the coil are both located outside the first cylinder; an electric heating jacket is provided on the outer wall of the first cylinder, and an outlet is provided on the side of the first cylinder. The outlet is connected to the inlet of the primary condenser, the outlet of the primary condenser is connected to the inlet of the secondary condenser, the outlet at the bottom of the secondary condenser is connected to the inlet of the product collection tank, and the outlet at the top of the secondary condenser is connected to the inlet at the bottom of the tail gas adsorption tower.

[0005] Furthermore, the primary condenser collector, the secondary condenser collector, and the product collection tank all include a second cylinder and a jacket for adjusting the temperature of the corresponding second cylinder. The jacket is connected to the corresponding second cylinder, and each jacket is provided with a refrigerant inlet and a refrigerant outlet.

[0006] Furthermore, a mass flow meter is also installed on the intake pipe to control the gas flow rate.

[0007] Furthermore, the agitator head extends to a position close to the bottom of the first cylinder.

[0008] Furthermore, the inlet of the primary condenser is located at the bottom of the primary condenser, and the outlet is located at the top of the primary condenser.

[0009] Furthermore, the inlet of the secondary condenser is located in the middle of the secondary condenser.

[0010] Furthermore, the inlet of the product collection tank is located at the top of the product collection tank.

[0011] Furthermore, a level gauge is installed on the side of the first cylinder of the reactor, the level gauge pipe is made of PFA material, and the gas disperser is located below the level line.

[0012] Furthermore, the first cylinder of the reactor is made of Monel or nickel, which reduces the risk of corrosion from fluorine gas.

[0013] Furthermore, the solid material includes some non-metallic inorganic substances such as arsenic, tellurium, and iodine, and some metallic powders such as iridium.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] (1) Solid material powder is dispersed in a solvent and then transferred to a reactor. The stirrer in the reactor ensures that the solid material is always in a dispersed state, which is more conducive to contact with fluorine gas and thus improves the reaction efficiency. Fluorine and nitrogen gas are continuously introduced into the reactor through the inlet and the flow rate is controlled by a mass flow meter. The fluorine and nitrogen gas are introduced into the reactor at a slow speed through the gas disperser, so as to be more fully dispersed. This greatly increases the contact probability and contact time between fluorine gas and metal powder. Fluorine gas reacts with metal in the solvent. The heat of reaction released by the reaction can be absorbed by the solvent. At the same time, the built-in coil and the two work together to control the reaction temperature, reduce the risk of side reactions, improve product purity, and to a certain extent avoid the decomposition of some metal high fluoride due to excessive heat released by the reaction. At the same time, a two-stage reaction device is designed so that some of the low fluoride produced by the reaction of metal with fluorine gas can be fluorinated again to form high fluoride, thereby further ensuring excess fluorine gas and obtaining high-yield transition metal high fluoride.

[0016] (2) Fluorine and nitrogen gas pass through a gas disperser, and the solid material is dispersed in the solution. The synergistic effect of both increases the probability of contact between the material and the fluorine gas, which is beneficial for the reaction. Simultaneously, the reaction of the solid material and fluorine gas in the solvent effectively absorbs some of the heat of reaction, preventing product decomposition due to excessively high temperatures. Combined with external temperature control, the reaction temperature can be precisely controlled. This prevents material from being carried by the gas into valves or pipelines, causing blockages. This reduces the high requirements of the reaction conditions on the entire equipment, laying a good foundation for its practical industrial production.

[0017] 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

[0018] Figure 1 This is a schematic diagram of the structure of a reaction device for reacting solid materials with fluorine gas according to this utility model.

[0019] Figure 2 This is a schematic diagram of the reactor structure in a reaction apparatus for reacting solid materials with fluorine gas according to this utility model.

[0020] Figure Labels

[0021] 1-Reactor, 2-First-stage condenser, 3-Second-stage condenser, 4-Product collection tank, 5-Tail gas adsorption tower, 11-First cylinder, 12-Inlet, 13-Outlet, 14-Inlet pipe, 15-Agitator, 16-Coil, 17-Gas disperser, 18-Mass flow meter, 19-Level gauge, 20-Electric heating jacket, 21-Inlet, 22-Inlet pipe. Detailed Implementation

[0022] To further illustrate the technical means and effects adopted by this utility model to achieve its intended purpose, the following detailed description, in conjunction with preferred embodiments and accompanying drawings, will describe in detail the specific implementation, structure, features, and effects of a reaction apparatus for reacting solid materials with fluorine gas according to this utility model.

[0023] In the description of this utility model, it should be understood that the terms "center", "upper", "lower", "front", "rear", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0024] Please combine Figure 1-2 An embodiment of a reaction apparatus for reacting solid materials with fluorine gas includes a reactor 1, a primary condenser 2, a secondary condenser 3, a product collection tank 4, and a tail gas adsorption tower 5. The reactor 1 includes a sealed first cylindrical body 11. An inlet pipe 14, a feed pipe 22, a stirrer 15, and a coil 16 are all installed at the top of the first cylindrical body 11. One end of the inlet pipe 14 outside the first cylindrical body 11 is the inlet 12, and the other end of the inlet pipe 14 extends through the top of the first cylindrical body 11 to a position near the bottom of the first cylindrical body 11. One end of the feed pipe 22 outside the first cylindrical body 11 is the feed inlet 21. An outlet 13 is provided on the side of the first cylindrical body 11. The outlet 13 connects to the primary condenser 2. The inlet of the first-stage condenser 2 is connected to the inlet of the second-stage condenser 3. The outlet of the second-stage condenser 3 at the bottom is connected to the inlet of the product collection tank 4. The outlet of the second-stage condenser 3 at the top is connected to the inlet at the bottom of the tail gas adsorption tower 5. The first-stage condenser 2, the second-stage condenser 3, and the product collection tank 4 all include a second cylinder and a jacket for adjusting the temperature of the corresponding second cylinder. The jacket is connected to the corresponding second cylinder, and each jacket is provided with a refrigerant inlet and a refrigerant outlet.

[0025] The inlet of the first-stage condenser 2 is located at the bottom of the first-stage condenser 2, and the outlet is located at the top of the first-stage condenser 2.

[0026] The inlet of the secondary condenser collector 3 is located in the middle of the secondary condenser collector 3.

[0027] The inlet of product collection tank 4 is located at the top of product collection tank 4.

[0028] A gas disperser 17 is installed at the end of the inlet pipe 14 near the bottom of the first cylinder 11. A mass flow meter 18 is also installed on the inlet pipe 14. Fluorine and nitrogen gas continuously enter the reactor through the inlet 12, and the flow rate is controlled by the mass flow meter. The gas disperser 17 then fully disperses the gas into the reactor. The stirring head of the agitator 15 extends to a position near the bottom of the first cylinder 11. The inlet and outlet of the coil 16 are both located at the top of the first cylinder 11, meaning that the inlet and outlet of the coil 16 are located outside the first cylinder 11. This is used to introduce circulating condensate water to absorb the heat of reaction generated by the raw materials in the reactor.

[0029] A level gauge 19 is installed on the side of the first cylindrical body 11 of reactor 1 to observe the liquid level. The level gauge pipe is made of PFA material. The gas disperser 17 is located below the liquid level line.

[0030] The first cylinder 11 of reactor 1 is made of Monel or nickel material, which reduces the risk of fluorine gas corrosion to the reactor.

[0031] The reactor 1 is heated by an electric heating jacket 20 disposed on the outer wall of the first cylinder 11.

[0032] In use, the device of this invention disperses solid powder in a solvent and adds it to reactor 1 through inlet 22. The solution is then at the liquid level line. Reactor 1 is then sealed and a leak test is performed. After reactor 1 is airtight, fluorine-nitrogen gas is introduced through inlet 12. The fluorine-nitrogen gas is fully dispersed by gas disperser 17. At the same time, stirrer 15 can ensure the dispersion of solid powder in the solution and prevent solid powder deposition. The electric heating jacket 20 is turned on to heat the solid material and react with fluorine gas in the solvent. The heat of reaction released by the reaction is first absorbed by the solvent and then condensed and circulated by the built-in coil 16 to control the temperature, which can prevent the metal high fluoride from decomposing due to excessive temperature. The upper space of reactor 1 retains unreacted fluorine gas. On the one hand, it can continue to react with the raw materials to improve the utilization rate of fluorine gas. On the other hand, it can react with low-fluoride compounds to convert them into high-fluoride compounds, which is beneficial to improving the purity of the product. The mixed gas containing high-fluoride compounds first enters the primary condenser 2 through the outlet 13, then enters the secondary condenser 3, and is finally collected in the product collection tank 4. The non-condensable excess gases such as fluorine and nitrogen enter the tail gas adsorption tower 5 through the upper outlet of the secondary condenser 3, and are discharged after adsorption treatment.

[0033] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Any simple modifications, equivalent changes, and alterations made by those skilled in the art to the above embodiments based on the technical essence of the present utility model without departing from the scope of the present utility model's technical solution shall still fall within the scope of the present utility model's technical solution.

Claims

1. A reaction apparatus for reacting solid materials with fluorine gas, characterized in that, The system includes a reactor, a primary condenser, a secondary condenser, a product collection tank, and a tail gas adsorption tower. The reactor comprises a sealed first cylinder, with an inlet pipe, a feed pipe, a stirrer, and a coil all extending through the top of the first cylinder. The inlet pipe has an inlet at one end outside the first cylinder and extends through the top of the first cylinder to a position near the bottom of the first cylinder. A gas disperser is located at the end of the inlet pipe near the bottom of the first cylinder. The feed pipe has a feed inlet at one end outside the first cylinder. The inlet and outlet of the coil are both located outside the first cylinder. An electric heating jacket is provided on the outer wall of the first cylinder. An outlet is located on the side of the first cylinder, which is connected to the inlet of the primary condenser. The outlet of the primary condenser is connected to the inlet of the secondary condenser. The outlet of the secondary condenser at the bottom is connected to the inlet of the product collection tank. The outlet of the secondary condenser at the top is connected to the inlet at the bottom of the tail gas adsorption tower.

2. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The primary condenser, secondary condenser, and product collection tank all include a second cylinder and a jacket for adjusting the temperature of the corresponding second cylinder. The jacket is connected to the corresponding second cylinder, and each jacket is provided with a refrigerant inlet and a refrigerant outlet.

3. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The intake pipe is also equipped with a mass flow meter for controlling the gas flow rate.

4. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The agitator head extends to a position close to the bottom of the first cylinder.

5. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The inlet of the primary condenser is located at the bottom of the primary condenser, and the outlet is located at the top of the primary condenser.

6. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The inlet of the secondary condenser is located in the middle of the secondary condenser.

7. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The inlet of the product collection tank is located at the top of the product collection tank.

8. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, A level gauge is installed on the side of the first cylinder of the reactor, and the gas disperser is located below the level line.

9. The reaction apparatus for reacting solid materials with fluorine gas as described in claim 1, characterized in that, The first cylinder of the reactor is made of Monel or nickel.

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