Method and device for continuously producing sulfuryl fluoride

Abstract

The invention relates to a method and a device for continuously producing sulfuryl fluoride. The method is a gas-solid reaction among reaction raw materials, does not need to use a solvent and a catalyst, is high in production efficiency, short in production period, high in sulfuryl fluoride yield and low in production cost, and can realize continuous production.

Description

Technical Field

[0001] This application relates to the field of chemical engineering technology, and specifically relates to a method and device for continuously producing sulfuryl fluoride. Background Art

[0002] Sulfuryl fluoride is one of the important raw materials for producing lithium battery electrolytes. Currently, sulfuryl fluoride is usually prepared by an intermittent process in the presence of a catalyst and an optional solvent. This method has low production efficiency, a long production cycle, low sulfuryl fluoride yield, and high production cost. Summary of the Invention

[0003] In view of the problems in the background art, this application provides a method for continuously producing sulfuryl fluoride. This method does not require the use of a solvent and a catalyst, has high production efficiency, a short production cycle, high sulfuryl fluoride yield, and low production cost, and can achieve continuous production.

[0004] The method for continuously producing sulfuryl fluoride provided in the first aspect of this application includes the following steps:

[0005] Continuously introduce a fluorinated salt powder and gaseous sulfuryl chloride into a fluidized boiling bed reactor to make the fluorinated salt powder in a fluidized boiling state, keep the temperature of the fluidized boiling bed reactor at 100 - 200 °C, and cause a gas-solid reaction between sulfuryl chloride and the fluorinated salt;

[0006] Collect the gaseous product and separate the gaseous product to obtain sulfuryl fluoride.

[0007] In this application, the fluorinated salt powder is in a fluidized boiling state in gaseous sulfuryl chloride. The fluorinated salt and sulfuryl chloride are in full contact and can fully undergo a gas-solid reaction at high temperature, with high reaction efficiency and high sulfuryl fluoride yield. In addition, this application does not require the use of a catalyst and a solvent, and does not involve the deactivation of the catalyst, so continuous production can be achieved, improving production efficiency and reducing the production cycle. In addition, the raw materials used in this application are only sulfuryl chloride and fluorinated salt, with low production cost, and the by-product is a chloride salt, with few by-products. In addition, compared with the industrial preparation of sulfuryl fluoride, the method for preparing sulfuryl fluoride in this application avoids the use of dangerous materials such as hydrogen fluoride and chlorine gas, with high safety.

[0008] In some embodiments, according to the first aspect, the first example of the first aspect is proposed. The temperature of the fluidized boiling bed reactor is 150 - 200 °C, preferably 170 - 200 °C.

[0009] By optimizing the gas-solid reaction temperature, it is beneficial to improve the reaction efficiency and the sulfuryl fluoride yield.

[0010] In some embodiments, according to the first aspect, the second example of the first aspect is proposed. The pressure of the gas-solid reaction is 0 - 0.2 Mpa, preferably 0.15 - 0.2 Mpa.

[0011] By optimizing the gas-solid reaction pressure, it is beneficial to improve the reaction efficiency and increase the yield of sulfuryl fluoride.

[0012] In some embodiments, according to the first aspect, a third example of the first aspect is proposed. The molar ratio of sulfuryl chloride to fluoride salt introduced per unit time is 1:(2 - 3).

[0013] By optimizing the molar ratio of reaction raw materials, it is beneficial to promote the full progress of the gas-solid reaction, and improve the reaction efficiency, raw material utilization rate, as well as the yield and purity of sulfuryl fluoride, etc.

[0014] In some embodiments, according to the first aspect, a fourth example of the first aspect is proposed. Before entering the fluidized bed reactor, the fluoride salt powder is preheated to 100 - 200 °C.

[0015] The reaction temperature in the fluidized bed reactor is 100 - 200 °C. Preheating the fluoride salt powder before introducing it into the fluidized bed reactor is beneficial to maintaining a constant temperature in the fluidized bed reactor, avoiding the liquefaction of gaseous sulfuryl chloride due to the temperature reduction in the fluidized bed reactor, which may cause the fluoride salt powder to agglomerate, not conducive to the full progress of the gas-solid reaction, and reducing the reaction efficiency and the yield of sulfuryl fluoride.

[0016] In some embodiments, according to the first aspect, a fifth example of the first aspect is proposed. The D50 particle size of the fluoride salt powder is below 100 μm.

[0017] By optimizing the D50 particle size of the fluoride salt powder, it is beneficial to increase the gas-solid contact area, make mass transfer more sufficient, and further beneficial to the full progress of the gas-solid reaction, improving the reaction efficiency and the yield of sulfuryl fluoride.

[0018] In some embodiments, according to the first aspect, a sixth example of the first aspect is proposed. The fluoride salt includes one or more of sodium fluoride, potassium fluoride, ammonium fluoride, sodium fluoride, potassium fluoride, silver fluoride, antimony trifluoride, potassium bifluoride, cesium fluoride.

[0019] These fluoride salts can all react with gaseous sulfuryl chloride to form sulfuryl fluoride. Among them, potassium fluoride and sodium fluoride are more likely to obtain fine powder and have low cost.

[0020] In some embodiments, according to the first aspect, a seventh example of the first aspect is proposed. The separation includes gas-solid separation; and optionally gas-gas separation.

[0021] The gaseous products discharged from the fluidized bed reactor may include powder. After gas-solid separation, the powder can be removed to improve the purity of the gaseous products. In addition, the gaseous products after gas-solid separation may contain unreacted gaseous sulfuryl chloride and by-product sulfuryl fluoride chloride. Therefore, through gas-gas separation, the unreacted gaseous sulfuryl chloride and by-product sulfuryl fluoride chloride can be removed, thereby improving the purity of sulfuryl fluoride.

[0022] The second aspect of the present application provides a device for continuously producing sulfuryl fluoride, comprising:

[0023] A gas storage tank, provided with a gas outlet;

[0024] A solid powder storage tank, provided with a discharging opening;

[0025] A fluidized boiling bed reactor, the upper part of the fluidized boiling bed reactor is provided with a feeding opening and a gaseous product outlet, the bottom is provided with an air inlet and a discharging opening, the air inlet is arranged above the discharging opening and is connected with the gas outlet of the gas storage tank, and the feeding opening is connected with the discharging opening of the solid powder storage tank;

[0026] A separation unit, the separation unit is connected with the gaseous product outlet of the fluidized boiling bed reactor.

[0027] In the present application, gaseous thionyl chloride is introduced from the bottom of the fluidized boiling bed reactor. By using the upward flow of the gas, the fluorinated salt powder fed from the upper part of the fluidized boiling bed reactor tumbles up and down, that is, in a fluidized boiling state, so that the powder is evenly distributed in the reaction zone. On the one hand, the agglomeration of the powder is reduced, and local caking is reduced. On the other hand, the contact opportunity between the powder and the gas is increased, so that the reaction between the raw materials is more thorough, and the reaction efficiency and product yield are improved.

[0028] In some embodiments, according to the second aspect, a first example of the second aspect is proposed. The fluidized boiling bed reactor includes a gas-solid two-phase fluidized boiling bed reactor.

[0029] By using the gas-solid two-phase fluidized boiling bed reactor, the gas-solid reaction can be fully carried out, and the reaction effect can be improved.

[0030] In some embodiments, according to the second aspect, a second example of the second aspect is proposed. The device of the present application further includes: a sulfuryl fluoride buffer tank, a compressor and a sulfuryl fluoride storage tank connected in sequence. The sulfuryl fluoride buffer tank is connected with the separation unit. The pressure of the sulfuryl fluoride buffer tank is preferably 0 - 0.05 Mpa lower than the pressure of the fluidized boiling bed reactor.

[0031] The compressor can compress the sulfuryl fluoride in the buffer tank into the storage tank to become liquid sulfuryl fluoride, reduce the volume of the storage tank, and is beneficial to storage and transportation.

[0032] In some embodiments, according to the second aspect, a third example of the second aspect is proposed. The separation unit includes a dust filter.

[0033] By using the dust filter, gas-solid separation can be realized, and the powder in the gaseous product can be removed.

[0034] In some embodiments, according to the second aspect, a fourth example of the second aspect is proposed. The dust filter includes:

[0035] The first dust filter, the top of the first dust filter is connected to the gaseous product outlet of the fluidized boiling bed reactor; the bottom of the first dust filter is preferably connected to the bottom of the fluidized boiling bed reactor;

[0036] The second dust filter; the bottom of the second dust filter is connected to the top of the first dust filter.

[0037] After the preliminary gas-solid separation is carried out by the first dust filter, and then the deep gas-solid separation is carried out by the second dust filter, which is beneficial to reducing the powder content in sulfuryl fluoride and improving the purity of sulfuryl fluoride.

[0038] In some embodiments, according to the second aspect, the fifth example of the second aspect is proposed, and the separation unit further includes a condenser. The condenser is connected to the top of the dust filter.

[0039] When the gaseous thionyl chloride does not fully participate in the reaction and / or when sulfuryl fluoride chloride by-products are generated, the condensation function of the condenser can be used to liquefy the gaseous thionyl chloride and sulfuryl fluoride chloride into liquids, so as to separate them from the gaseous sulfuryl fluoride.

[0040] In some embodiments, according to the second aspect, the sixth example of the second aspect is proposed, and the number of fluidized boiling bed reactors and separation units is the same and both are more than 2. The fluidized boiling bed reactors and the separation units are connected alternately in sequence.

[0041] Connecting multiple fluidized boiling bed reactors in series to form a multi-stage reaction is beneficial to improving the conversion rate of reaction raw materials, so that the reaction raw materials and the intermediate product sulfuryl fluoride chloride can participate in the reaction as completely as possible. In the case of complete reaction, the condenser can be not used for gas-gas separation. However, in order to improve the purity of sulfuryl fluoride, a condenser is usually used to remove impurities as much as possible.

[0042] In some embodiments, according to the second aspect, the seventh example of the second aspect is proposed, and the device of the present application further includes: a thionyl chloride storage tank and a preheater connected thereto. The preheater is connected to the gas storage tank. The outer wall of the gas storage tank is preferably provided with a heat preservation jacket.

[0043] The thionyl chloride liquid is transported from the storage tank to the preheater for heating, vaporized and then transported to the gas storage tank for standby. The heat preservation jacket on the outer wall of the gas storage tank can play a heat preservation effect, keeping the thionyl chloride in a gaseous state and reducing the liquefaction phenomenon.

[0044] In some embodiments, according to the second aspect, the eighth example of the second aspect is proposed, and the device of the present application further includes: a solid powder heater. The solid powder heater is connected to the solid powder storage tank. The outer wall of the solid powder storage tank is preferably provided with a heat preservation jacket.

[0045] The fluorinated salt powder is heated in a solid powder heater and then transported to a solid powder storage tank for standby. The heat-insulating jacket on the outer wall of the solid powder storage tank can achieve a heat-insulating effect, making the temperature of the fluorinated salt powder the same as that in the fluidized boiling bed reactor, which is beneficial to the smooth progress of the gas-solid reaction in the fluidized boiling bed reactor and reduces the liquefaction phenomenon of sulfuryl chloride.

[0046] In some embodiments, according to the second aspect, a ninth example of the second aspect is proposed. A gas distribution pipe is further provided inside the fluidized boiling bed reactor. The gas distribution pipe is connected to the inlet of the fluidized boiling bed reactor. Distribution openings penetrating the pipe wall are provided on the gas distribution pipe. Preferably, the axis of the gas distribution pipe forms an angle with the axis of the fluidized boiling bed reactor, and the angle is greater than 0 and less than or equal to 90°. Preferably, the opening direction of the distribution opening forms an angle with the axis of the fluidized boiling bed reactor, and the angle is greater than 0 and less than or equal to 90°. Preferably, the distribution openings on the gas distribution pipe are symmetrically distributed.

[0047] By optimizing the gas inlet channel of gaseous sulfuryl chloride, the phenomenon of blockage of the inlet channel can be reduced.

[0048] In some embodiments, according to the second aspect, a tenth example of the second aspect is proposed. A feed valve is provided at the discharge opening of the solid powder storage tank. A first feeder is provided at the feed inlet of the fluidized boiling bed reactor. The first feeder is used to control the feeding speed.

[0049] The feeder can control the feeding speed of the fluorinated salt powder, which is beneficial to accurately controlling the dosage ratio between the reaction raw materials and promoting the full progress of the gas-solid reaction.

[0050] In some embodiments, according to the second aspect, an eleventh example of the second aspect is proposed. A second feeder, a discharge valve, a first level gauge, and a second level gauge are sequentially provided at the bottom of the fluidized boiling bed reactor from bottom to top.

[0051] The first and second level gauges are used to control the upper and lower limits of the powder level at the bottom to avoid excessive accumulation of powder at the bottom of the fluidized boiling bed reactor, which affects the progress of the gas-solid reaction.

[0052] The above description is only an overview of the technical solution of this application. In order to be able to understand the technical means of this application more clearly, it can be implemented according to the content of the specification. And in order to make the above and other purposes, features, and advantages of this application more obvious and understandable, the specific embodiments of this application are specifically exemplified below. BRIEF DESCRIPTION OF THE DRAWINGS

[0053] Various other advantages and benefits will become apparent to those of ordinary skill in the art by reading the following detailed description of the preferred embodiments. The drawings are only for the purpose of showing the preferred embodiments and are not considered to be a limitation of the present invention. Also, throughout the drawings, the same reference numerals are used to represent the same components. In the drawings:

[0054] Figure 1 It is a schematic structural diagram of a device for preparing sulfuryl fluoride in an embodiment of the present application.

[0055] Figure 2 It is a schematic structural diagram of a fluidized bed reactor and a first dust filter in an embodiment of the present application.

[0056] Figure 3 It is a projection diagram of the cross-section of a gas distribution pipe along the axial direction in an embodiment of the present application.

[0057] Description of reference numerals:

[0058] 1 - sulfuryl chloride storage tank, 2 - preheater, 3 - gas storage tank, 301 - gas supply pipe, 302 - mass flowmeter, 303 - intake valve, 4 - solid powder storage tank, 401 - feed valve, 402 - first feeder, 5 - fluidized bed reactor, 501 - second level gauge, 502 - first level gauge, 503 - discharge valve, 504 - second feeder, 505 - gas distribution pipe, 6 - first dust filter, 601 - output pipe, 602 - powder recovery pipe, 7 - second dust filter, 701 - connecting pipe, 702 - conveying pipeline, 703 - outlet valve, 8 - condenser, 9 - liquid storage tank, 10 - sulfuryl fluoride buffer tank, 11 - compressor, 12 - sulfuryl fluoride storage tank. Detailed embodiments

[0059] The following will describe in detail the embodiments of the technical solutions of the present application with reference to the drawings. The following embodiments are only used to more clearly illustrate the technical solutions of the present application and are therefore only examples and cannot be used to limit the protection scope of the present application.

[0060] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which this application belongs; the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" and any variations thereof in the specification and claims of this application and the above drawings are intended to cover non-exclusive inclusion.

[0061] In the description of the embodiments of the present application, technical terms such as "first" and "second" are only used to distinguish different objects, and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity, specific order or primary-secondary relationship of the indicated technical features. In the description of the embodiments of the present application, the meaning of "a plurality of" is more than two, unless otherwise specifically defined.

[0062] Reference to "embodiment" herein means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the present application. The phrase appears in various places in the specification and does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0063] In the description of the embodiments of the present application, the term "and / or" is merely a description of the association relationship of associated objects, indicating that three relationships can exist. For example, A and / or B can represent three situations: the existence of A, the simultaneous existence of A and B, and the existence of B.

[0064] In the description of the embodiments of the present application, the term "a plurality of" means more than two (including two). Similarly, "a plurality of groups" means more than two groups (including two groups), and "a plurality of pieces" means more than two pieces (including two pieces).

[0065] In the description of the embodiments of the present application, the orientation or positional relationship indicated by technical terms such as "up", "down", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the embodiments of the present application and simplifying the description, rather than indicating or implying that the indicated device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present application.

[0066] In the description of the embodiments of the present application, unless otherwise clearly specified and limited, technical terms such as "installation", "connection", "connection", "fixation", etc. should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can also be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and can be the communication inside two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the embodiments of the present application can be understood according to specific circumstances.

[0067] Sulfuryl fluoride is one of the important raw materials for producing lithium battery electrolytes. Currently, sulfuryl fluoride is usually prepared by an intermittent process using sulfuryl chloride and a fluorination reagent in the presence of a catalyst and an optional solvent. However, due to catalyst deactivation, the catalyst needs to be replaced regularly, making it difficult to achieve continuous production, resulting in low production efficiency, long production cycles, low sulfuryl fluoride yields, and high production costs.

[0068] Therefore, this application proposes a method for continuously producing sulfuryl fluoride. The method includes the following steps:

[0069] Continuously introduce a fluorinated salt powder and gaseous sulfuryl chloride into a fluidized boiling bed reactor to make the fluorinated salt powder in a fluidized boiling state, maintain the temperature of the fluidized boiling bed reactor at 100 - 200 °C, and cause the sulfuryl chloride to undergo a gas-solid reaction with the fluorinated salt;

[0070] Collect the gaseous product and separate the gaseous product to obtain sulfuryl fluoride.

[0071] In this application, the fluorinated salt powder is in a fluidized boiling state in gaseous sulfuryl chloride. The fluorinated salt and sulfuryl chloride are in full contact and can fully undergo a gas-solid reaction at high temperature, with high reaction efficiency and high sulfuryl fluoride yield. In addition, this application does not require the use of a catalyst and a solvent, does not involve catalyst deactivation, and thus can achieve continuous production, improve production efficiency, and reduce the production cycle. Moreover, the raw materials used in this application are only sulfuryl chloride and fluorinated salt, with low production costs, and the by-product is chloride salt, with few by-products. Additionally, compared with the industrial preparation of sulfuryl fluoride, the sulfuryl fluoride preparation method in this application avoids the use of dangerous materials such as hydrogen fluoride and chlorine, with high safety.

[0072] In this application, the "fluidized boiling state" refers to the powder particles constantly fluttering and tumbling in the flowing gas stream, being in a fluidized state, similar to a "boiling state". The fluorinated salt powder particles in the fluidized boiling state can be in full contact with gaseous sulfuryl chloride, fully mass transfer, and promote the full and effective progress of the gas-solid reaction.

[0073] In this application, the chemical reactions occurring in the fluidized boiling bed reactor are as follows:

[0074] SO2Cl2 + M1F → SO2FCl + M1Cl;

[0075] SO2FCl + M2F → SO2F2 + M2Cl.

[0076] The overall reaction formula is:

[0077] SO2Cl2 + 2MF → SO2F2 + 2MCl

[0078] Among them, in the above formula, M1F and M2F can be the same fluorinated salt or different fluorinated salts, and can be metal fluoride salts or non-metal fluoride salts. M1 and M2 refer to the cations combined with fluoride ions.

[0079] In some embodiments, the temperature of the fluidized boiling bed reactor can be 150 - 200 °C, preferably 170 - 200 °C.

[0080] In the absence of a catalyst and a solvent, gaseous sulfuryl chloride and solid fluoride salts can directly undergo a gas-solid reaction at high temperatures. By optimizing the gas-solid reaction temperature, it is beneficial to improve the reaction efficiency and the yield of sulfuryl fluoride.

[0081] In some specific embodiments, the temperature of the fluidized boiling bed reactor can be 100 °C, 110 °C, 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, 170 °C, 180 °C, 190 °C or 200 °C.

[0082] In some embodiments, the pressure of the gas-solid reaction can be 0 - 0.2 Mpa, preferably 0.15 - 0.2 Mpa.

[0083] By optimizing the gas-solid reaction pressure, it is beneficial to improve the reaction efficiency and the yield of sulfuryl fluoride.

[0084] In some specific embodiments, the pressure of the gas-solid reaction can be 0 Mpa, 0.01 Mpa, 0.02 Mpa, 0.04 Mpa, 0.06 Mpa, 0.08 Mpa, 0.1 Mpa, 0.12 Mpa, 0.14 Mpa, 0.16 Mpa, 0.18 Mpa or 0.2 Mpa.

[0085] In some embodiments, the molar ratio of sulfuryl chloride to fluoride salt introduced per unit time can be 1:(2 - 3).

[0086] By optimizing the molar ratio of the reaction raw materials, it is beneficial to promote the full progress of the gas-solid reaction, and improve the reaction efficiency, raw material utilization rate, as well as the yield and purity of sulfuryl fluoride, etc.

[0087] In some specific embodiments, the molar ratio of sulfuryl chloride to fluoride salt introduced per unit time can be 1:2, 1:2.1, 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1:2.6, 1:2.7, 1:2.8, 1:2.9 or 1:3.

[0088] In some embodiments, before entering the fluidized boiling bed reactor, the fluoride salt powder can be preheated to 100 - 200 °C.

[0089] The reaction temperature in the fluidized bed reactor is 100 - 200 °C. Preheating the fluorinated salt powder before introducing it into the fluidized bed reactor helps maintain a constant temperature inside the fluidized bed reactor, preventing the gaseous sulfuryl chloride from liquefying due to a decrease in temperature inside the fluidized bed reactor, which may cause the fluorinated salt powder to agglomerate and is not conducive to the full progress of the gas-solid reaction, reducing the reaction efficiency and the sulfuryl fluoride yield. The preheating temperature of the fluorinated salt powder can be the same as the temperature of the fluidized bed reactor.

[0090] In some specific embodiments, before entering the fluidized bed reactor, the fluorinated salt powder can be preheated to 100 °C, 110 °C, 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, 170 °C, 180 °C, 190 °C or 200 °C.

[0091] In some embodiments, the D50 particle size of the fluorinated salt powder can be 100 μm or less.

[0092] By optimizing the D50 particle size of the fluorinated salt powder, it is beneficial to increase the gas-solid contact area, make mass transfer more sufficient, and thus is conducive to the full progress of the gas-solid reaction, improving the reaction efficiency and the sulfuryl fluoride yield.

[0093] In some specific embodiments, the D50 particle size of the fluorinated salt powder can be 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm.

[0094] Optionally, the D50 particle size of the fluorinated salt powder can be 20 - 80 μm.

[0095] In some embodiments, the fluorinated salt includes one or more of sodium fluoride, potassium fluoride, ammonium fluoride, sodium fluoride, potassium fluoride, silver fluoride, antimony trifluoride, potassium bifluoride, cesium fluoride.

[0096] These fluorinated salts can all react with gaseous sulfuryl chloride to form sulfuryl fluoride. Among them, potassium fluoride and sodium fluoride are more likely to obtain fine powder and have low costs. In addition, the reaction effect of potassium fluoride is better than that of sodium fluoride, but potassium fluoride is more expensive than sodium fluoride.

[0097] In some embodiments, the separation includes gas-solid separation; and optional gas-gas separation

[0098] The gaseous products discharged from the fluidized boiling bed reactor may include powders. After gas-solid separation, the powders can be removed to improve the purity of sulfuryl fluoride. In addition, the gaseous products after gas-solid separation may still contain unreacted gaseous thionyl chloride and the by-product sulfuryl fluoride chloride. Therefore, the unreacted gaseous thionyl chloride and the by-product sulfuryl fluoride chloride can be removed through gas-gas separation, thereby improving the purity of sulfuryl fluoride. Whether to perform gas-gas separation can be selected according to the completeness of the gas-solid reaction. Generally, in order to ensure high purity of sulfuryl fluoride, gas-gas separation is carried out.

[0099] In some specific embodiments, taking advantage of the different boiling points of thionyl chloride (boiling point 69.1 °C), sulfuryl fluoride chloride (boiling point 5 °C) and sulfuryl fluoride (boiling point -55 °C), gas-gas separation can be carried out by condensation. The unreacted thionyl chloride and sulfuryl fluoride chloride are condensed into liquids, thus being separated from the gaseous sulfuryl fluoride. The condensation temperature can be -20 - 0 °C, such as -20 °C, -15 °C, -10 °C, -5 °C or 0 °C.

[0100] In some embodiments, before entering the fluidized boiling bed reactor, the temperature of gaseous thionyl chloride can be controlled at 100 °C - 200 °C, such as 100 °C, 110 °C, 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, 170 °C, 180 °C, 190 °C or 200 °C.

[0101] Controlling the temperature of the reaction raw materials before entering the fluidized boiling bed reactor to be the same as or close to the temperature inside the fluidized boiling bed reactor is beneficial to the efficient progress of the gas-solid reaction.

[0102] In some embodiments, the feeding rate of gaseous thionyl chloride can be 35 - 40 kg / h, such as 35 kg / h, 36 kg / h, 37 kg / h, 38 kg / h, 39 kg / h or 40 kg / h.

[0103] The thionyl chloride gas passes through the inside of the cylinder of the fluidized boiling bed reactor from bottom to top, so that the feeding rate of the gaseous thionyl chloride is greater than or equal to the particle critical fluidization velocity, and the fluorinated salt powder tumbles up and down, that is, in a "boiling" state. By optimizing the feeding rate and the feeding rate of the reaction raw materials, it is beneficial to make the fluorinated salt powder in a fluidized boiling state, increase the gas-solid contact area, and improve the reaction efficiency.

[0104] The second aspect of the present application provides a device for continuously producing sulfuryl fluoride, including:

[0105] A gas storage tank with an air outlet;

[0106] A solid powder storage tank with a discharging port;

[0107] A fluidized boiling bed reactor, with a feed inlet and a gaseous product outlet provided at the upper part of the fluidized boiling bed reactor, and an air inlet and a discharge outlet provided at the bottom. The air inlet is arranged above the discharge outlet and is connected to the outlet of a gas storage tank, and the feed inlet is connected to the discharge opening of a solid powder storage tank;

[0108] A separation unit, which is connected to the gaseous product outlet of the fluidized boiling bed reactor.

[0109] In this application, gaseous sulfuryl chloride is introduced from the bottom of the fluidized boiling bed reactor. By utilizing the upward flow of the gas, the fluorinated salt powder fed from the upper part of the fluidized boiling bed reactor tumbles up and down, that is, it is in a fluidized boiling state, so that the powder is evenly distributed in the reaction zone. On the one hand, it reduces the agglomeration of the powder and reduces the formation of local lumps. On the other hand, it increases the contact opportunity between the powder and the gas, makes the reaction between the raw materials more thorough, and improves the reaction efficiency and product yield.

[0110] Figure 1 The structural schematic diagram of the device for preparing sulfuryl fluoride in an embodiment of this application is given. Figure 2 The structural schematic diagram of the fluidized boiling bed reactor and the first dust filter in an embodiment of this application is given. As Figure 1-2 shown, the fluorinated salt powder enters the fluidized boiling bed reactor 5 through the feed inlet at the upper part of the fluidized boiling bed reactor 5. There is no special limitation on the specific position of the feed inlet, which can be set on the top wall of the fluidized boiling bed reactor 5 or on the side wall of the fluidized boiling bed reactor 5.

[0111] The gas storage tank 3 is connected to the fluidized boiling bed reactor 5 through a gas supply pipe 301. A mass flowmeter 302 and an intake valve 303 are provided on the gas supply pipe 301 to control the flow rate of sulfuryl chloride gas. The sulfuryl chloride gas enters from the bottom of the fluidized boiling bed reactor 5 and passes through the inside of the fluidized boiling bed reactor 5 from bottom to top, making the fluorinated salt powder fed from the upper part of the fluidized boiling bed reactor 5 in a fluidized boiling state. The fluidized boiling bed reactor 5 can be heated by heat transfer oil or high-pressure steam.

[0112] In some embodiments, the fluidized boiling bed reactor 5 includes a gas-solid two-phase fluidized boiling bed reactor.

[0113] By using the gas-solid two-phase fluidized boiling bed reactor, the gas-solid reaction can be fully carried out and the reaction effect can be improved.

[0114] In some embodiments, the device of this application further includes: a sulfuryl fluoride buffer tank 10, a compressor 11 and a sulfuryl fluoride storage tank 12 connected in sequence. The sulfuryl fluoride buffer tank 10 is connected to the separation unit. The pressure of the sulfuryl fluoride buffer tank 10 is preferably 0 - 0.05 Mpa lower than the pressure of the fluidized boiling bed reactor 5.

[0115] The compressor can compress sulfuryl fluoride in the buffer tank into the storage tank, turning it into liquid sulfuryl fluoride, reducing the volume of the storage tank, which is beneficial for storage and transportation. The frequency of the compressor 11 can be automatically frequency-converted according to the pressure of the sulfuryl fluoride buffer tank 10.

[0116] The pressure of the fluidized boiling bed reactor 5 is slightly greater than that of the sulfuryl fluoride buffer tank 10, which is beneficial for the gas to flow towards the sulfuryl fluoride buffer tank 10 through the pressure difference.

[0117] There is a certain amount of sulfuryl fluoride stored in the sulfuryl fluoride buffer tank 10, which can play a buffering role and reduce the adverse impact on the gas-gas separation effect when the compressor pumps air.

[0118] In some embodiments, the separation unit includes a dust filter.

[0119] The dust filter can be used to achieve gas-solid separation and remove the powder in the gaseous product.

[0120] In some embodiments, the dust filter includes:

[0121] The first dust filter 6, the top of the first dust filter 6 is connected to the gaseous product outlet of the fluidized boiling bed reactor 5;

[0122] The second dust filter 7; the bottom of the second dust filter 7 is connected to the top of the first dust filter 6.

[0123] After the preliminary gas-solid separation is carried out by the first dust filter 6, the second dust filter 7 is used for in-depth gas-solid separation, which is beneficial for reducing the powder content in sulfuryl fluoride and improving the purity of sulfuryl fluoride.

[0124] In some specific embodiments, the bottom of the first dust filter 6 is preferably connected to the bottom of the fluidized boiling bed reactor 5. For example, the bottom of the first dust filter 6 is connected to the bottom of the fluidized boiling bed reactor 5 through the powder recovery pipe 602.

[0125] After the first dust filter 6 performs gas-solid separation, powder will accumulate at the bottom. These powders may contain sodium chloride generated after the reaction and unreacted sodium fluoride powder. By connecting the bottom of the first dust filter 6 to the bottom of the fluidized boiling bed reactor 5, the powder accumulated at the bottom can be transported to the bottom of the fluidized boiling bed reactor 5 for unified discharge, which can simplify the equipment and reduce costs.

[0126] In some specific embodiments, the first dust filter 6 is connected to the gaseous product outlet of the fluidized boiling bed reactor 5 through the output pipe 601. The bottom of the second dust filter 7 can be connected to the top of the first dust filter 6 through the connecting pipe 701.

[0127] In some specific embodiments, the first dust filter 6 may include a cyclone separator. The second dust filter 7 may include a bag filter.

[0128] In some embodiments, the separation unit further includes a condenser 8. The condenser 8 is connected to the top of the dust filter.

[0129] In the case where gaseous thionyl chloride does not fully participate in the reaction and / or thionyl fluorochloride by-products are generated, the condensation function of the condenser 8 can be used to liquefy gaseous thionyl chloride and thionyl fluorochloride into liquids, so as to separate them from gaseous sulfuryl fluoride. The sulfuryl fluoride obtained after gas-gas separation has a high purity and can be transported to backend equipment such as a sulfuryl fluoride buffer tank 10, and compressed to a sulfuryl fluoride storage tank 12 for storage by a compressor 11.

[0130] The condenser 8 can be connected to the dust filter through a delivery pipeline 702. In some specific embodiments, the condenser 8 can be connected to the top of the second dust filter 7 through the delivery pipeline 702. An outlet valve 703 can be provided on the delivery pipeline 702 for controlling gas delivery.

[0131] In some specific embodiments, a liquid storage tank 9 can be provided downstream of the bottom of the condenser 8. The liquid storage tank 9 can be connected to the bottom of the condenser 8 through a connection pipeline for containing the liquid discharged from the condenser. The liquid may contain unreacted thionyl chloride and thionyl fluorochloride by-products. These liquids can be transported to the front end to be re-vaporized and then enter the fluidized boiling bed reactor 5 to continue the reaction, realizing recycling, reducing pollutant emissions, and reducing costs.

[0132] In some embodiments, the number of fluidized boiling bed reactors and separation units is the same and both are more than 2. The fluidized boiling bed reactors and separation units are alternately connected in sequence.

[0133] To simplify the equipment, the separation unit here may include a dust filter but does not include a condenser.

[0134] After the gaseous product discharged from the first-stage fluidized boiling bed reactor enters the first-stage separation unit for gas-solid separation, the obtained gas may still contain unreacted thionyl chloride and thionyl fluorochloride by-products. To make full use of this part of substances, a second-stage fluidized boiling bed reactor and a second-stage separation unit can be connected in series after the first-stage separation unit. The top of the first-stage separation unit can be connected to the inlet of the second-stage fluidized boiling bed reactor to re-introduce the gas containing unreacted thionyl chloride and thionyl fluorochloride by-products into the fluidized boiling bed reactor to continue the reaction. After the reaction, the gaseous product can be discharged to the second-stage separation unit for gas-solid separation, and so on. The number of stages of the fluidized boiling bed reactor or the number of fluidized boiling bed reactors can be set according to actual needs, for example, it can be 2 or 3. The structure of each stage of the fluidized boiling bed reactor can be the same, and the structure of each stage of the separation unit can be the same.

[0135] Connecting multiple fluidized boiling bed reactors in series to form a multi-stage reaction is beneficial to improving the conversion rate of reaction raw materials, enabling the reaction raw materials and intermediate product sulfuryl fluoride chloride to participate in the reaction as completely as possible. In the case of complete reaction, a condenser can be not used for gas-gas separation. However, in order to improve the purity of sulfuryl fluoride, a condenser is usually used to remove impurities as much as possible.

[0136] In some embodiments, the device of the present application further includes: a sulfuryl chloride storage tank 1 and a preheater 2 connected thereto. The preheater 2 is connected to a gas storage tank 3. The outer wall of the gas storage tank 3 is preferably provided with a heat-insulating jacket.

[0137] The sulfuryl chloride liquid is transported from the storage tank to the preheater for heating, vaporized and then transported to the gas storage tank for standby. The heat-insulating jacket on the outer wall of the gas storage tank can play a heat-insulating effect, keeping the sulfuryl chloride in a gaseous state and reducing the liquefaction phenomenon.

[0138] In some embodiments, the device of the present application further includes: a solid powder heater (not shown in the figure). The solid powder heater is connected to a solid powder storage tank 4. The outer wall of the solid powder storage tank 4 is preferably provided with a heat-insulating jacket.

[0139] The fluorinated salt powder is heated in the solid powder heater and then transported to the solid powder storage tank 4 for standby. The heat-insulating jacket on the outer wall of the solid powder storage tank 4 can play a heat-insulating effect, making the temperature of the fluorinated salt powder the same as the temperature inside the fluidized boiling bed reactor 5, which is beneficial to the smooth progress of the gas-solid reaction inside the fluidized boiling bed reactor 5 and reduces the sulfuryl chloride liquefaction phenomenon.

[0140] In some embodiments, as Figure 2 shown, a gas distribution pipe 505 is further provided inside the fluidized boiling bed reactor. The gas distribution pipe 505 is connected to the air inlet of the fluidized boiling bed reactor. As Figure 3 shown, the gas distribution pipe 505 is provided with distribution ports penetrating the pipe wall. Preferably, the axis of the gas distribution pipe 505 forms an angle with the axis of the fluidized boiling bed reactor 5, and the angle is greater than 0 and less than or equal to 90°. Preferably, the opening direction of the distribution port forms an angle with the axis of the fluidized boiling bed reactor, and the angle is greater than 0 and less than or equal to 90°. Preferably, the distribution ports on the gas distribution pipe 505 are symmetrically distributed.

[0141] The sulfuryl chloride gas from the gas supply pipe 301 enters the inside of the fluidized boiling bed reactor 5 through the distribution ports on the gas distribution pipe 505. In order to reduce the occurrence of blockage of the air inlet channel, the setting mode of the gas distribution pipe 505 and the distribution ports can be optimized, thereby reducing the powder from entering the air inlet channel and causing blockage.

[0142] In some specific embodiments, the gas distribution pipe 505 is horizontally arranged. The opening direction of the distribution ports on the pipe wall of the gas distribution pipe 505 forms an angle equal to or close to 90° with the axis of the fluidized boiling bed reactor 5. Such an arrangement can maximally avoid powder from entering the intake passage and causing blockage.

[0143] In some embodiments, a feed valve 401 is provided at the discharge opening of the solid powder storage tank 4. A first feeder 402 is provided at the feed opening of the fluidized boiling bed reactor 5. The first feeder 402 is used to control the feeding speed.

[0144] The first feeder 402 is connected to the feed valve 401 and can control the feeding speed of the fluoride powder, which is beneficial to accurately controlling the dosage ratio between the reaction raw materials and promoting the full progress of the gas-solid reaction. In addition, the first feeder 402 also has the function of dispersing the fluoride powder, which is beneficial to fluidizing and boiling the powder.

[0145] In some specific embodiments, the first feeder 402 includes a star feeder.

[0146] In some embodiments, a second feeder 504, a discharge valve 503, a first level gauge 502, and a second level gauge 501 are successively provided at the bottom of the fluidized boiling bed reactor 5 from bottom to top.

[0147] The discharge speed of the powder in the fluidized boiling bed reactor 5 is controlled by the frequency of the second feeder 504. When the fluoride enters the fluidized boiling bed reactor and reacts with the gaseous sulfuryl chloride, the generated chloride salt and the unreacted fluoride powder first fill the bottom of the fluidized boiling bed reactor until the powder submerges the first level gauge 502. At this time, the discharge valve 503 is opened and the rotation speed of the second feeder 504 is controlled for discharging. When the powder touches the second level gauge 501, the discharge frequency of the second feeder 504 is increased.

[0148] The first and second level gauges are used to control the upper and lower limit values of the powder level at the bottom, so as to avoid excessive powder accumulation at the bottom of the fluidized boiling bed reactor and affect the progress of the gas-solid reaction.

[0149] In some specific embodiments, each of the first and second level gauges may include a rotary vane level gauge.

[0150] In some specific embodiments, an opening is preferably provided on the side wall of the fluidized boiling bed reactor between the first level gauge 502 and the discharge valve 503. The opening is connected to the bottom of the separation unit through a powder recovery pipe 602.

[0151] Providing an opening on the side wall of the fluidized boiling bed reactor between the first level gauge 502 and the discharge valve 503 and conveying the powder from the separation unit to the bottom of the fluidized boiling bed reactor for unified discharge can simplify the equipment and reduce the cost.

[0152] In some embodiments, the fluidized boiling bed reactor includes, from bottom to top, a first cylindrical section, a first conical section, a second cylindrical section, and a second conical section that are sequentially connected and coaxial. The diameter of the second cylindrical section is greater than that of the first cylindrical section.

[0153] As Figure 2 shown, the first cylindrical section is provided with a second feeder 504 and a discharge valve 503. The first conical section is provided with a first level gauge 502 and a second level gauge 501. The gas distribution pipe 505 can be arranged above the junction of the first conical section and the second cylindrical section.

[0154] Embodiment

[0155] Hereinafter, embodiments of the present application will be described. The embodiments described below are exemplary and are only used to explain the present application and should not be construed as a limitation to the present application. For those embodiments where specific technologies or conditions are not indicated, the technologies or conditions described in the literature in this field or according to the product specifications are followed. For reagents or instruments whose manufacturers are not indicated, they are all conventional products that can be obtained through commercial purchase.

[0156] Embodiment 1

[0157] In Figure 1 and 2 the device shown, sulfuryl fluoride is produced. The specific production process is as follows.

[0158] (1) Preheating stage: The sodium fluoride powder with a D50 particle size of 55 μm is heated to 180 °C and stored in the solid powder storage tank 4 while maintaining the temperature. The liquid sulfuryl chloride in the sulfuryl chloride storage tank 1 is vaporized into a gas through the preheater 2 and stored in the gas storage tank 3.

[0159] (2) Feeding stage: The gaseous sulfuryl chloride in the gas storage tank 3 is transported to the fluidized boiling bed reactor 3 through the gas supply pipe 301, and the feeding rate of the gaseous sulfuryl chloride is controlled to be 38 kg / h by using a mass flow meter 302 and an intake valve 303. The feeding valve 401 on the solid powder storage tank 4 is opened, and the rotation speed of the first feeder 402 (star feeder) is controlled, so as to control the sodium fluoride in the solid powder storage tank 4 to enter the fluidized boiling bed reactor 5 at a feeding rate of 26 kg / h. After regulation, the molar ratio of sulfuryl chloride to fluoride salt introduced per unit time is 1:2.2.

[0160] (3) Reaction stage: The temperature of the fluidized boiling bed reactor 5 is controlled to be 180 °C, and the pressure is 0.17 Mpa. The pressure can be controlled by the outlet valve 703 behind the second dust filter 7 (bag filter). In the fluidized boiling bed reactor 5, sulfuryl chloride reacts with sodium fluoride to form sulfuryl fluoride.

[0161] (4) Separation stage: The gas after the reaction passes through the first dust filter 6 (cyclone separator) and the second dust filter 7 (bag filter) to separate the powder from the gas. The separated mixed gas is further separated by the condenser 8 to obtain sulfuryl fluoride gas. After the pressure of the sulfuryl fluoride gas reaches 0.12 Mpa in the sulfuryl fluoride buffer tank 10, it is compressed by the compressor 11 and sent to the sulfuryl fluoride storage tank 12.

[0162] Examples 2 - 5

[0163] It is carried out according to the method described in Example 1, except that the temperature of the fluidized boiling bed reactor is different from that in Example 1, as shown in Table 1 below.

[0164] Table 1

[0165] Number Fluidized boiling bed reactor temperature °C Example 1 180 Example 2 170 Example 3 150 Example 4 200 Example 5 100

[0166] Examples 6 - 9

[0167] It is carried out according to the method described in Example 1, except that the pressure of the fluidized boiling bed reactor is different from that in Example 1, as shown in Table 2 below.

[0168] Table 2

[0169] Number Fluidized boiling bed reactor pressure Mpa Example 1 0.17 Example 6 0.15 Example 7 0.2 Example 8 0.01 Example 9 0.3

[0170] Examples 10 - 13

[0171] It is carried out according to the method described in Example 1, except that the molar ratio of sulfuryl chloride to fluoride salt introduced per unit time is different from that in Example 1, as shown in Table 3 below.

[0172] Table 3

[0173]

[0174] Examples 14 - 16

[0175] It is carried out according to the method described in Example 1, except that the D50 particle size of the sodium fluoride powder is different from that in Example 1, as shown in Table 4 below.

[0176] Table 4

[0177] Number D50 particle size μm Example 1 55 Example 14 100 Example 15 20 Example 16 150

[0178] Examples 17 - 18

[0179] It is carried out according to the method described in Example 1, except that the type of fluoride salt is different from that in Example 1, as shown in Table 5 below.

[0180] Table 5

[0181] Number Type of fluoride salt Example 1 Sodium fluoride Example 17 Potassium fluoride Example 18 Sodium fluoride and potassium fluoride (mass ratio 1:1)

[0182] Comparative Examples 1-2

[0183] It was carried out according to the method described in Example 1, except that the temperature of the fluidized boiling bed reactor was different from that in Example 1, as shown in Table 6 below.

[0184] Table 6

[0185]

[0186]

[0187] The purity and yield of the gaseous sulfuryl fluoride prepared in the above examples and comparative examples were analyzed, and the residual amount of fluoride salt was analyzed. The results are shown in Table 7 below.

[0188] Test for the residual amount of fluoride salt:

[0189] Weigh 0.1 g of the powder from the 504 - second feeder. After completely dissolving and making up the volume to 250 ml, the fluoride ion concentration C in the solution was quantitatively detected by ion chromatography. Then, the mass concentration of fluoride ions in the powder was calculated, and further the mass content of fluoride salt in the powder was deduced. Among them, the calculation formula for the mass concentration of fluoride ions in the powder is W F- = C * V / m × 100%, where C is the F ion concentration (unit μg / ml), V is the made-up volume (unit ml) (here it is 250 ml), and m is the mass of the weighed powder (unit g) (here it is 0.1 g).

[0190] Table 7

[0191]

[0192]

[0193] It can be seen from Table 7 that by using the device and method of the present application, sulfuryl fluoride can be continuously produced without using solvents and catalysts, with high production efficiency, short production cycle, high yield and purity of sulfuryl fluoride, and low production cost.

[0194] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention should be covered by the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A method for continuously producing sulfuryl fluoride, characterized in that, It includes the following steps: Continuously introduce fluorinated salt powder and gaseous sulfuryl chloride into the fluidized boiling bed reactor to make the fluorinated salt powder in a fluidized boiling state, keep the temperature of the fluidized boiling bed reactor at 100 - 200 °C, and cause a gas-solid reaction between sulfuryl chloride and the fluorinated salt; Collect the gaseous product and separate the gaseous product to obtain sulfuryl fluoride.

2. The method according to claim 1, wherein The temperature of the fluidized boiling bed reactor is 150 - 200 °C, preferably 170 - 200 °C.

3. The method according to claim 1 or 2, characterized in that, The pressure of the gas-solid reaction is 0 - 0.2 Mpa, preferably 0.15 - 0.2 Mpa.

4. The method according to any one of claims 1 to 3, characterized in that The molar ratio of sulfuryl chloride to fluorinated salt introduced per unit time is 1:(2 - 3).

5. The method according to any one of claims 1-4, characterized in that, Before entering the fluidized boiling bed reactor, preheat the fluorinated salt powder to 100 - 200 °C.

6. The method according to any one of claims 1-5, characterized in that, The particle size D50 of the fluorinated salt powder is below 100 μm.

7. The method according to any one of claims 1-6, characterized in that, The fluorinated salt includes one or more of sodium fluoride, potassium fluoride, ammonium fluoride, sodium fluoride, potassium fluoride, silver fluoride, antimony trifluoride, potassium bifluoride, cesium fluoride.

8. The method according to any one of claims 1-7, characterized in that, The separation includes gas-solid separation; and optionally gas-gas separation.

9. An apparatus for continuously producing sulfuryl fluoride, characterized in that, It includes: A gas storage tank provided with an air outlet; A solid powder storage tank provided with a discharge port; A fluidized boiling bed reactor, the upper part of the fluidized boiling bed reactor is provided with a feed port and a gaseous product outlet, the bottom is provided with an air inlet and a discharge port, the air inlet is arranged above the discharge port and is connected to the air outlet of the gas storage tank, and the feed port is connected to the discharge port of the solid powder storage tank; A separation unit, the separation unit is connected to the gaseous product outlet of the fluidized boiling bed reactor.

10. The device according to claim 9, characterized in that, The fluidized boiling bed reactor includes a gas-solid two-phase fluidized boiling bed reactor.

11. The device according to claim 9 or 10, characterized in that, It also includes: a sulfuryl fluoride buffer tank, a compressor and a sulfuryl fluoride storage tank connected in sequence, the sulfuryl fluoride buffer tank is connected to the separation unit; the pressure of the sulfuryl fluoride buffer tank is preferably 0 - 0.05 Mpa lower than the pressure of the fluidized boiling bed reactor.

12. The device according to any one of claims 9-11, characterized in that, The separation unit includes a dust filter.

13. The device according to claim 12, characterized in that, The dust filter includes: A first dust filter, the top of the first dust filter is connected to the gaseous product outlet of the fluidized boiling bed reactor; the bottom of the first dust filter is preferably connected to the bottom of the fluidized boiling bed reactor; A second dust filter; the bottom of the second dust filter is connected to the top of the first dust filter.

14. The device according to claim 12 or 13, characterized in that, The separation unit also includes a condenser, and the condenser is connected to the top of the dust filter.

15. The device according to any one of claims 9 - 13, characterized in that, The number of the fluidized boiling bed reactors and the separation units is the same and both are more than 2, and the fluidized boiling bed reactors and the separation units are connected alternately in sequence.

16. The device according to any one of claims 9 - 15, characterized in that, It also includes: A sulfuryl chloride storage tank and a preheater connected thereto, the preheater is connected to the gas storage tank; the outer wall of the gas storage tank is preferably provided with a heat preservation jacket.

17. The device according to any one of claims 9 - 16, characterized in that It also includes: A solid powder heater, the solid powder heater is connected to the solid powder storage tank; the outer wall of the solid powder storage tank is preferably provided with a heat preservation jacket.

18. The device according to any one of claims 9-17, characterized in that, A gas distribution pipe is further provided inside the fluidized boiling bed reactor. The gas distribution pipe is connected to the air inlet of the fluidized boiling bed reactor, and distribution openings penetrating the pipe wall are provided on the gas distribution pipe. Preferably, an included angle is formed between the axis of the gas distribution pipe and the axis of the fluidized boiling bed reactor, and the included angle is greater than 0 and less than or equal to 90°. Preferably, an included angle is formed between the opening direction of the distribution opening and the axis of the fluidized boiling bed reactor, and the included angle is greater than 0 and less than or equal to 90°. Preferably, the distribution openings on the gas distribution pipe are symmetrically distributed.

19. The device according to any one of claims 9-18, characterized in that, A feed valve is provided at the discharge opening of the solid powder storage tank, and a first feeder is provided at the feed inlet of the fluidized boiling bed reactor. The first feeder is used to control the feeding speed.

20. The device according to any one of claims 9-19, characterized in that, A second feeder, a discharge valve, a first level gauge, and a second level gauge are sequentially provided at the bottom of the fluidized boiling bed reactor from bottom to top.

Images