A method for the continuous production of sulfuryl fluoride in a fluidized bed

Abstract

The application belongs to the technical field of sulfuric fluoride preparation method, and particularly relates to a method for continuously preparing sulfuric fluoride in a fluidized bed, which comprises the following steps: S1, using carbon tetrafluoride as a working gas, adopting plasma pretreatment on a hydrogen fluoride-amine complex for standby; S2, preheating the fluidized bed to 150-180 DEG C, adding fluorinated salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, and heating to 190-200 DEG C; after gasification, preheating sulfuric chloride to 100-120 DEG C, and then introducing into the fluidized bed for two-stage heating reaction; S3, gas-solid separation, washing and drying the gas, and thus sulfuric fluoride is obtained. The application combines plasma treatment with the fluidized bed, improves the synthesis efficiency, reduces the generation of by-products, and improves the product purity.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of sulfuryl fluoride preparation method, and particularly relates to a method for continuously preparing sulfuryl fluoride in a fluidized bed. BACKGROUND

[0002] Sulfuryl fluoride is used in lithium battery electrolyte, fumigant and fluorine-containing drug synthesis, and the preparation methods of sulfuryl fluoride include direct synthesis method, oxidation method and fluorination agent conversion.

[0003] The direct synthesis method uses sulfur dioxide (SO2) and fluorine gas (F2) as raw materials to react to generate sulfuryl fluoride under the action of a catalyst. This method has mild reaction conditions and high product purity, but the flow of fluorine gas needs to be strictly controlled to avoid side reactions. In industry, activated carbon or metal fluoride (such as CoF3) is often used as a catalyst, and the reaction temperature is controlled at 100-150℃, and the conversion rate can reach more than 90%. However, fluorine gas is used in this method, which is highly dangerous.

[0004] The oxidation method is to prepare sulfuryl fluoride by reacting thionyl chloride (SOCl2) with hydrogen fluoride (HF) or fluorinated salt (such as KF). This method avoids the direct use of highly dangerous fluorine gas and is more suitable for small-scale synthesis in the laboratory.

[0005] The fluorination agent conversion method uses thionyl chloride (SO2Cl2) to react with a fluorination agent (such as AgF2) to generate sulfuryl fluoride through chlorine-fluorine exchange. This method has high selectivity, but the cost is high, and it is suitable for the preparation of high-purity sulfuryl fluoride. The recovery of metal fluoride also needs to be solved.

[0006] Through research, a Chinese patent with application number CN202210110583.8 discloses a method for efficiently preparing sulfuryl fluoride by using thionyl chloride fluorination method. Solvent and hydrogen fluoride complex are added to the reaction kettle, the reaction system is cooled to below 10℃, and then thionyl chloride is added dropwise under normal pressure and the temperature of the reaction system is controlled below 60℃ to obtain sulfuryl fluoride.

[0007] This method can reduce the production cost of sulfuryl fluoride, improve the purity and yield of sulfuryl fluoride, and produce less waste during production, which is suitable for industrial production. However, the purification step of the product in this scheme is relatively complicated. SUMMARY

[0008] The purpose of the present application is to provide a method for continuously preparing sulfuryl fluoride in a fluidized bed, which combines plasma treatment with a fluidized bed to improve synthesis efficiency, reduce the production of by-products, and improve product purity.

[0009] The technical problem of the present application is solved by using the following technical scheme.

[0010] In one aspect, the embodiment of the present application provides a method for preparing sulfuryl fluoride in a fluidized bed, comprising the following steps:

[0011] S1, using carbon tetrafluoride as working gas, plasma pretreating hydrogen fluoride-amine complex;

[0012] S2, preheating the fluidized bed to 150-180℃, adding fluorinated salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, heating to 190-200℃; preheating sulfuryl chloride to 100-120℃ after gasification, and then introducing into the fluidized bed for two-stage heating reaction;

[0013] S3, gas-solid separation, the gas is washed and dried to obtain sulfuryl fluoride.

[0014] In some embodiments of the present application, in step S1, the power of plasma treatment is 100-200W, the treatment time is 10-30min, and the introduction rate of carbon tetrafluoride is 20-50sccm.

[0015] In some embodiments of the present application, the hydrogen fluoride-amine complex is a molecular sieve loaded hydrogen fluoride-amine complex, which is prepared by the following method:

[0016] Mixing activated molecular sieve with anhydrous toluene, condensing refluxing for 12 hours, and vacuum drying,

[0017] Dissolving diisopropylethylamine trifluoride in anhydrous toluene to obtain an impregnation solution;

[0018] Dropping the impregnation solution into the molecular sieve, ultrasonic dispersion, reduced pressure distillation, and drying to obtain the hydrogen fluoride-amine complex.

[0019] In some embodiments of the present application, the mass fraction of the impregnation solution is 20-30%.

[0020] In some embodiments of the present application, the mass ratio of the molecular sieve to the impregnation solution is 3:1, and the impregnation treatment temperature is 0-5℃.

[0021] In some embodiments of the present application, the molecular sieve is 4A or 5A molecular sieve, and the pore size is 0.4-0.5nm.

[0022] In some embodiments of the present application, the ultrasonic dispersion power is 10-20KHz, and the dispersion time is 10-20min.

[0023] In some embodiments of the present application, in step S2, the temperature of the first-stage heating is 180-200℃, and the temperature of the second-stage heating is 250-350℃.

[0024] Compared with the prior art, the present application has the following beneficial effects:

[0025] The application uses sulfuryl chloride and hydrogen fluoride-amine complex as raw materials, cooperates plasma and fluidized bed, improves the synthesis efficiency of sulfuryl fluoride, reduces the generation of side reactions, and improves the purity of the product. The fluidized bed design realizes continuous feeding of raw materials and continuous output of products, and the production capacity is increased by 30-40% compared with the fixed bed.

[0026] Carbon tetrafluoride is used as working gas, and hydrogen fluoride-amine complex is pretreated by plasma, so that C-F bonds can be constructed on the surface of hydrogen fluoride-amine complex, the reaction activity of fluorine atoms is improved, and the occurrence of side reactions is reduced; and the micro-nano rough structure formed increases the contact area of the reaction. BRIEF DESCRIPTION OF DRAWINGS

[0027] In order to more clearly illustrate the technical solutions of the embodiments of the application, the following will briefly introduce the drawings needed to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the application, and therefore should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.

[0028] Figure 1 The gas chromatogram of sulfuryl fluoride in the second embodiment of the application;

[0029] Figure 2 The gas chromatogram of sulfuryl fluoride in the second embodiment of the application; DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the embodiments of the application more clear, the technical solutions in the embodiments of the application will be clearly and completely described below. If the specific conditions are not specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer are used. If the reagents or instruments used are not specified by the manufacturer, they are all conventional products that can be purchased on the market.

[0031] It should be noted that the embodiments in the application and the features in the embodiments can be combined with each other without conflict. The application will be described in detail below with reference to specific embodiments.

[0032] The embodiments of the application provide a method for continuously preparing sulfuryl fluoride in a fluidized bed, comprising the following steps:

[0033] S1, using carbon tetrafluoride as working gas, pretreating hydrogen fluoride-amine complex by plasma, standby; the power of plasma treatment is 100-200 W, the treatment time is 10-30 min, and the input rate of carbon tetrafluoride is 20-50 sccm;

[0034] S2, preheat the fluidized bed to 150-180℃, add the fluorinated salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, heat to 190-200℃; after gasification, preheat the sulfuryl chloride to 100-120℃, then pass into the fluidized bed for two-stage heating reaction; the temperature of the first-stage heating is 180-200℃; the temperature of the second-stage heating is 250-350℃.

[0035] In the fluidized bed, the hydrogen fluoride-amine complex (DIPEA·3HF) and the gasified sulfuryl chloride (SO2Cl2) undergo a gas-solid reaction at 250-350℃: SO2Cl2+2[R3N·HF]→SO2F2+2[R3N·HCl], the chlorine atoms in the sulfuryl chloride are replaced by fluorine atoms to generate sulfuryl fluoride (SO2F2), and the byproduct is organic amine hydrochloride. The second-stage heating temperature (250-350℃) can accelerate the fluorine substitution rate, improve the conversion rate, and make the conversion rate > 90%. The fluorinated salt can supply fluorine source for the reaction and improve the total conversion rate of the sulfuryl chloride.

[0036] S3, gas-solid separation, the gas is washed and dried, and sulfuryl fluoride is obtained.

[0037] The hydrogen fluoride-amine complex is prepared in the following method:

[0038] The activated molecular sieve is mixed with anhydrous toluene, and condensation reflux is performed for 12 hours, and the molecular sieve is dried in vacuum, the molecular sieve is 4A or 5A molecular sieve, and the pore size is 0.4-0.5nm;

[0039] The diisopropylethylamine trihydrofluoride is dissolved in anhydrous toluene to obtain an impregnation solution, and the mass fraction of the impregnation solution is 20-30%;

[0040] The impregnation solution is added dropwise into the molecular sieve, ultrasonic dispersion is performed, vacuum distillation is performed, and drying is performed, and the hydrogen fluoride-amine complex is obtained. The power of the ultrasonic dispersion is 10-20KHz, and the dispersion time is 10-20min. The mass ratio of the molecular sieve to the impregnation solution is 3:1, and the impregnation treatment temperature is 0-5℃.

[0041] The diisopropylethylamine trihydrofluoride is loaded on the molecular sieve through the impregnation method, the porous structure of the molecular sieve can increase the contact area of the sulfuryl chloride and the diisopropylethylamine trihydrofluoride, improve the reaction efficiency, and reduce the generation of byproducts.

[0042] In the embodiments of the present application, the fluorinated salt is one or more of sodium fluoride, potassium fluoride and barium fluoride.

[0043] The features and performances of the present application are further described in detail in combination with the embodiments.

[0044] Embodiment one

[0045] Sulfuryl fluoride is synthesized in the following method:

[0046] 1. Preparation of hydrogen fluoride-amine complex

[0047] 5A type molecular sieve (pore size 0.5 nm) was selected, calcined at 550℃ for 6 hours to remove adsorbed water and impurities, and activated molecular sieve was obtained; the activated molecular sieve was mixed with anhydrous toluene, and condensed reflux was carried out for 12 hours; after centrifugal separation, vacuum drying was carried out at 110℃;

[0048] Diisopropylethylamine trifluoride was dissolved in anhydrous toluene to obtain an impregnation solution, and the mass fraction of the impregnation solution was 30%;

[0049] The impregnation solution was added to the molecular sieve at a mass ratio of 3:1, ultrasonic dispersion was carried out for 10 min, and the power of ultrasonic dispersion was 10KHz; then the impregnation system was transferred to a rotary evaporator, and the solvent was removed by vacuum distillation at 40℃, and dried in a vacuum oven at 60℃ for 12 hours, to obtain hydrogen fluoride-amine complex.

[0050] 2. Synthesis of sulfuryl fluoride in a fluidized bed

[0051] S1, using carbon tetrafluoride as working gas, hydrogen fluoride-amine complex was pretreated by plasma, and was ready for use; wherein the power of plasma treatment was 100W, the treatment time was 30min, and the input rate of carbon tetrafluoride was 20sccm;

[0052] S2, the fluidized bed was preheated to 150℃, and the pretreated hydrogen fluoride-amine complex and barium fluoride powder were added to the fluidized bed by carrier gas (helium), and heated to 190℃; after gasification, sulfuryl chloride was preheated to 100℃, and was input into the fluidized bed at a speed of 7g / min to carry out two-stage heating reaction; the temperature of the first-stage heating was 200℃; the temperature of the second-stage heating was 250℃; wherein the flow rate of carrier gas helium was 3.5L / min, and the pretreated hydrogen fluoride-amine complex and barium fluoride powder were input into the fluidized bed reactor at a speed of 17g / min.

[0053] S3, gas-solid separation (cyclone separation), the gas was washed and dried (calcium chloride drying), and sulfuryl fluoride was obtained.

[0054] Example two

[0055] Sulfuryl fluoride was synthesized by the following method:

[0056] 1. Preparation of hydrogen fluoride-amine complex

[0057] Select 5A molecular sieve (pore size 0.5 nm), calcined at 550 ℃ for 4 hours, remove adsorbed water and impurities, get activated molecular sieve; The activated molecular sieve and anhydrous toluene were mixed, and the condensation reflux was carried out for 12 hours. After centrifugal separation, vacuum drying was carried out at 110 ℃;

[0058] Dissolve diisopropyl ethylamine trifluoride in anhydrous toluene to obtain an impregnation solution, and the mass fraction of the impregnation solution is 20%;

[0059] According to the mass ratio of molecular sieve to impregnation solution of 3:1, the impregnation solution was added to the molecular sieve, ultrasonic dispersion was carried out for 10 min, and the power of ultrasonic dispersion was 20 KHz. Then the impregnation system was transferred to a rotary evaporator, and the solvent was removed by vacuum distillation at 40 ℃. Drying was carried out in a vacuum oven at 60 ℃ for 12 hours, and hydrogen fluoride-amine complex was obtained.

[0060] 2. Synthesis of sulfuryl fluoride in a fluidized bed

[0061] S1, using carbon tetrafluoride as working gas, using plasma pretreatment hydrogen fluoride-amine complex, standby; wherein, the power of plasma treatment is 200 W, the treatment time is 10 min, the input rate of carbon tetrafluoride is 50 sccm;

[0062] S2, preheat the fluidized bed to 150 ℃, add potassium fluoride powder and pretreated hydrogen fluoride-amine complex into the fluidized bed through carrier gas (helium), and heat to 190 ℃; After gasification, sulfuryl chloride is preheated to 100 ℃, and is input into the fluidized bed at a speed of 7 g / min to carry out two-stage heating reaction; The temperature of the first-stage heating is 200 ℃; The temperature of the second-stage heating is 350 ℃; The flow rate of carrier gas helium is 3.5 L / min, and the input speed of potassium fluoride powder and pretreated hydrogen fluoride-amine complex into the fluidized bed reactor is 17 g / min;

[0063] S3, gas-solid separation (cyclone separation), the gas is washed and dried (calcium chloride drying), and sulfuryl fluoride is obtained.

[0064] Example three

[0065] Sulfuryl fluoride is synthesized by the following method:

[0066] 1. Preparation of hydrogen fluoride-amine complex

[0067] Select 5A molecular sieve (pore size 0.5 nm), calcined at 550 ℃ for 6 hours, remove adsorbed water and impurities, get activated molecular sieve; The activated molecular sieve and anhydrous toluene were mixed, and the condensation reflux was carried out for 12 hours. After centrifugal separation, vacuum drying was carried out at 110 ℃;

[0068] The diisopropylethylamine trifluoride is dissolved in anhydrous toluene to obtain an impregnation solution, and the mass fraction of the impregnation solution is 25%;

[0069] The impregnation solution is added to the molecular sieve at a mass ratio of 3:1, ultrasonic dispersion is performed for 20 min, the power of ultrasonic dispersion is 10 KHz; then the impregnation system is transferred to a rotary evaporator, the solvent is removed by distillation under reduced pressure at 40°C, and drying is performed in a vacuum oven at 60°C for 12 hours, to obtain a hydrogen fluoride-amine complex.

[0070] 2. Synthesis of sulfuryl fluoride in a fluidized bed

[0071] S1, the hydrogen fluoride-amine complex is pretreated by plasma with carbon tetrafluoride as working gas; wherein the power of plasma treatment is 100 W, the treatment time is 30 min, and the input rate of carbon tetrafluoride is 50 sccm;

[0072] S2, the fluidized bed is preheated to 150°C, calcium fluoride powder and the pretreated hydrogen fluoride-amine complex are added to the fluidized bed through a carrier gas (helium), and heating is performed to 190°C; after gasification, sulfuryl chloride is preheated to 100°C, and is input into the fluidized bed at a speed of 7 g / min to perform a two-stage heating reaction; the temperature of the first-stage heating is 180°C; the temperature of the second-stage heating is 250°C; the flow rate of the carrier gas helium is 3.5 L / min, and the calcium fluoride powder and the pretreated hydrogen fluoride-amine complex are input into the fluidized bed reactor at a speed of 17 g / min.

[0073] S3, gas-solid separation (cyclone separation), the gas is washed and dried (calcium chloride drying), to obtain sulfuryl fluoride.

[0074] Example Four

[0075] Sulfuryl fluoride is synthesized by the following method:

[0076] 1. Preparation of hydrogen fluoride-amine complex

[0077] 5A type molecular sieve (pore size 0.5 nm) is selected, is calcined at 550°C for 6 hours to remove adsorbed water and impurities, to obtain activated molecular sieve; the activated molecular sieve is mixed with anhydrous toluene, and is condensed to reflux for 12 hours, is centrifuged and separated, and is dried at 110°C in a vacuum;

[0078] The diisopropylethylamine trifluoride is dissolved in anhydrous toluene to obtain an impregnation solution, and the mass fraction of the impregnation solution is 20%;

[0079] The impregnation liquid is added to the molecular sieve according to a mass ratio of 3:1, ultrasonic dispersion is performed for 20 min, and the ultrasonic dispersion power is 10 KHz; then the impregnation system is transferred to a rotary evaporator, the solvent is removed by distillation under reduced pressure at 40 DEG C, and drying is performed in a vacuum oven at 60 DEG C for 12 hours, thereby obtaining a hydrogen fluoride-amine complex.

[0080] 2. Synthesizing sulfuryl fluoride in a fluidized bed

[0081] S1, using carbon tetrafluoride as a working gas, the hydrogen fluoride-amine complex is pretreated by plasma, and is ready for use; wherein the plasma treatment power is 200 W, the treatment time is 20 min, and the carbon tetrafluoride input rate is 50 sccm;

[0082] S2, the fluidized bed is preheated to 180 DEG C, the calcium fluoride powder and the pretreated hydrogen fluoride-amine complex are added to the fluidized bed by a carrier gas (helium), and heating is performed to 190 DEG C; the sulfuryl chloride is preheated to 100 DEG C after gasification, and is input to the fluidized bed at a speed of 7 g / min, and a two-stage heating reaction is performed; the first-stage heating temperature is 180 DEG C; the second-stage heating temperature is 250 DEG C; the carrier gas helium flow rate is 3.5 L / min, and the potassium fluoride powder and the pretreated hydrogen fluoride-amine complex are input to the fluidized bed reactor at a speed of 17 g / min.

[0083] S3, gas-solid separation (cyclone separation), the gas is washed and dried (calcium chloride drying), thereby obtaining sulfuryl fluoride.

[0084] Example Five

[0085] Sulfuryl fluoride is synthesized by the following method:

[0086] 1. Preparing a hydrogen fluoride-amine complex

[0087] 5A type molecular sieve (pore size 0.5 nm) is selected, is calcined at 550 DEG C for 6 hours, and adsorbed water and impurities are removed, thereby obtaining activated molecular sieve; the activated molecular sieve is mixed with anhydrous toluene, and is condensed and refluxed for 12 hours, is centrifugally separated, and is dried in a vacuum oven at 110 DEG C;

[0088] Diisopropylethylamine trifluoride is dissolved in anhydrous toluene, thereby obtaining an impregnation liquid, and the mass fraction of the impregnation liquid is 30%;

[0089] The impregnation liquid is added to the molecular sieve according to a mass ratio of 3:1, ultrasonic dispersion is performed for 20 min, and the ultrasonic dispersion power is 10 KHz; then the impregnation system is transferred to a rotary evaporator, the solvent is removed by distillation under reduced pressure at 40 DEG C, and drying is performed in a vacuum oven at 60 DEG C for 12 hours, thereby obtaining a hydrogen fluoride-amine complex.

[0090] 2. Synthesizing sulfuryl fluoride in a fluidized bed

[0091] S1, using carbon tetrafluoride as the working gas, the hydrogen fluoride-amine complex was pretreated by plasma; wherein the power of the plasma treatment was 200 W, the treatment time was 10 min, and the flow rate of the carbon tetrafluoride was 20 sccm;

[0092] S2, the fluidized bed was preheated to 180℃, the calcium fluoride powder and the pretreated hydrogen fluoride-amine complex were added to the fluidized bed by the carrier gas (helium), and heated to 200℃; after gasification, the sulfuryl chloride was preheated to 100℃, and was introduced into the fluidized bed at a speed of 7 g / min to carry out a two-stage heating reaction; the temperature of the first-stage heating was 180℃; the temperature of the second-stage heating was 250℃; the flow rate of the carrier gas helium was 3.5 L / min, and the calcium fluoride powder and the pretreated hydrogen fluoride-amine complex were input into the fluidized bed reactor at a speed of 17 g / min.

[0093] S3, gas-solid separation (cyclone separation), the gas was washed and dried (calcium chloride drying), and sulfuryl fluoride was obtained.

[0094] Comparative Example One

[0095] The difference from Example One is that no plasma treatment is performed in step S1, and the remaining steps and raw materials are the same as those of Example One.

[0096] Comparative Example Two

[0097] The difference from Example One is that the diisopropylethylamine hydrogen fluoride complex is directly added in step S1 without being loaded on the molecular sieve, and the remaining steps and raw materials are the same as those of Example One.

[0098] Comparative Example Three

[0099] According to the method of Example One of patent CN117142436A, the fluidized bed reactor was preheated to 180℃, and the sulfuryl chloride was preheated to 120℃, then the flow rate of the carrier gas nitrogen was adjusted to 3.5 L / min, the potassium hydrogen fluoride was input into the fluidized bed reactor from the top of the fluidized bed by a solid feeder at a speed of 17 g / min along with the carrier gas, the sulfuryl chloride was sent into the fluidized bed reactor from the bottom of the fluidized bed by a liquid feeder at a speed of 6.9 g / min, the liquid feeder was first started, then the solid feeder was started, and then the solid and liquid materials were input into the fluidized bed reactor at the same time, respectively, the product generated by the reaction was sequentially subjected to a gas-solid separation device (cyclone separator) and a gas separation device (gas cryogenic separator), and then the gas phase obtained after the gas separation was washed and dried in a calcium chloride packed column to obtain sulfuryl fluoride.

[0100] It should be noted that the 5A molecular sieve used in the above examples and comparative examples is HTMS-5A spherical molecular sieve produced by Liaoning Haitai Technology Development Company, and the pore size is 0.5 nm.

[0101] Experimental Examples

[0102] The purity of the sulfuryl fluoride of Examples 1 to 3 and Comparative Examples 1 to 3 was detected by gas chromatography, and the results are shown in Table 1 and Figure 1 and Figure 2 .

[0103] Table 1

[0104]

[0105] As can be seen from the data in Table 1, the purity of the sulfuryl fluoride obtained by the preparation method of Examples 1 to 5 is higher; in Comparative Example 1, the diisopropylethylamine hydrogen fluoride complex is not subjected to plasma treatment, and its surface does not form C-F bonds, and it has fewer active fluorine atoms, which is prone to produce by-products and reduce the purity of the product; in Comparative Example 2, a molecular sieve carrier is not used, and the contact area of gaseous sulfuryl chloride with the diisopropylethylamine hydrogen fluoride complex in the fluidized bed is smaller than that of Example 1, which reduces the reaction efficiency, and it is more prone to produce by-products, and the purity of the product is also reduced accordingly.

[0106] In summary, the present application uses sulfuryl chloride and hydrogen fluoride-amine complex as raw materials, and cooperates with plasma and fluidized bed to improve the synthesis efficiency of sulfuryl fluoride, reduce the generation of side reactions, and improve the purity of the product; the fluidized bed design realizes continuous feeding of raw materials and continuous output of products, and the production capacity is increased by 30-40% compared with the fixed bed.

[0107] Carbon tetrafluoride is used as a working gas, and the hydrogen fluoride-amine complex is pretreated by plasma to construct C-F bonds on the surface of the hydrogen fluoride-amine complex, which improves the reactivity of fluorine atoms and reduces the occurrence of side reactions; at the same time, the micro-nano rough structure formed increases the contact area of the reaction.

[0108] The above-described embodiments are part of the embodiments of the present application, but not all of the embodiments. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but only represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of protection of the present application.

Claims

1. A method for the continuous production of sulfuryl fluoride in a fluidized bed, characterized in that, The method comprises the following steps: S1, using carbon tetrafluoride as working gas, plasma pretreats hydrogen fluoride-amine complex; S2, preheats the fluidized bed to 150-180℃, adds fluorinated salt powder and pretreated hydrogen fluoride-amine complex into the fluidized bed, heats to 190-200℃; preheats gaseous sulfuryl chloride to 100-120℃, then passes into the fluidized bed to carry out two-stage heating reaction; S3, gas-solid separation, washes and dries the gas to obtain sulfuryl fluoride; The hydrogen fluoride-amine complex is a molecular sieve loaded hydrogen fluoride-amine complex, which is prepared by the following method: Mixes activated molecular sieve with anhydrous toluene, condenses reflux for 12 hours, and vacuum dries, Dissolves diisopropylethylamine trifluoride in anhydrous toluene to obtain impregnation solution; Drops the impregnation solution into the molecular sieve, ultrasonically disperses, reduces pressure distillation, and dries to obtain the hydrogen fluoride-amine complex.

2. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, In step S1, the power of plasma treatment is 100-200W, the treatment time is 10-30min, and the passing rate of carbon tetrafluoride is 20-50sccm.

3. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, The mass fraction of the impregnation solution is 20-30%.

4. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, The mass ratio of the molecular sieve to the impregnation solution is 3:1, and the impregnation treatment temperature is 0-5℃.

5. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, The molecular sieve is 4A or 5A molecular sieve, and the pore size is 0.4-0.5nm.

6. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, The ultrasonic dispersion power is 10-20KHz, and the dispersion time is 10-20min.

7. The method of claim 1, wherein the fluidized bed continuous production of sulfuryl fluoride is characterized by, In step S2, the first-stage heating temperature is 180-200℃, and the second-stage heating temperature is 250-350℃.

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