Method for continuously preparing sulfuryl fluoride through fluidized bed

Abstract

The invention belongs to the technical field of sulfuryl fluoride preparation methods, and particularly relates to a method for continuously preparing sulfuryl fluoride by a fluidized bed, which comprises the following steps: S1, by taking carbon tetrafluoride as working gas, pretreating a hydrogen fluoride-amine complex by adopting plasma for later use; s2, preheating a fluidized bed to 150-180 DEG C, adding fluoride salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, and heating to 190-200 DEG C; preheating the gasified sulfuryl chloride to 100-120 DEG C, and introducing the preheated sulfuryl chloride into the fluidized bed for two-stage heating reaction; and S3, carrying out gas-solid separation, and washing and drying the gas to obtain sulfuryl fluoride. The plasma treatment is combined with the fluidized bed, so that the synthesis efficiency is improved, the generation of byproducts is reduced, and the product purity is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of sulfuryl fluoride preparation methods, and specifically relates to a method for continuously preparing sulfuryl fluoride in a fluidized bed. Background Art

[0002] Sulfuryl fluoride is used in the synthesis of lithium battery electrolytes, fumigants and fluorine-containing drugs. The preparation methods of sulfuryl fluoride include direct synthesis, oxidation, fluorination agent conversion, etc.

[0003] The direct synthesis method uses sulfur dioxide (SO2) and fluorine (F2) as raw materials, reacting in the presence of a catalyst to produce sulfuryl fluoride. This method offers mild reaction conditions and high product purity, but requires strict control of the fluorine flow rate to avoid side reactions. In industry, activated carbon or metal fluorides (such as CoF3) are commonly used as catalysts. With reaction temperatures controlled at 100-150°C, conversion rates exceeding 90% can be achieved. However, this method involves the use of fluorine gas, which is highly hazardous.

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

[0005] The fluorinating agent conversion method uses sulfuryl chloride (SO₂Cl₂) to react with a fluorinating agent (such as AgF₂) to produce sulfuryl fluoride through a chlorine-fluorine exchange process. This method is highly selective but relatively expensive. While suitable for the preparation of high-purity sulfuryl fluoride, it also requires addressing the issue of metal fluoride recovery.

[0006] After searching, Chinese patent application number CN202210110583.8 discloses an efficient method for preparing sulfuryl fluoride using the sulfuryl chloride fluorination method. A solvent and a hydrogen fluoride complex are added to a reactor, the reaction system is cooled to below 10°C, and sulfuryl chloride is added dropwise under normal pressure while controlling the temperature of the reaction system to below 60°C to obtain sulfuryl fluoride.

[0007] This method can reduce the production cost of sulfuryl fluoride, improve the purity and yield of sulfuryl fluoride, and generate less three wastes during the production process, making it suitable for industrial production. However, in this scheme, the purification steps of the product are relatively cumbersome. Summary of the Invention

[0008] The object of the present invention is to provide a method for continuously preparing sulfuryl fluoride in a fluidized bed, which combines plasma treatment with a fluidized bed, thereby improving synthesis efficiency, reducing the generation of by-products, and improving product purity.

[0009] The present invention solves the technical problem by adopting the following technical solutions.

[0010] On the one hand, an embodiment of the present invention provides a method for continuously preparing sulfuryl fluoride in a fluidized bed, comprising the following steps: S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for use; S2, preheating the fluidized bed to 150-180°C, adding the fluoride salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, and heating to 190-200°C; preheating the vaporized sulfuryl chloride to 100-120°C, and then introducing it into the fluidized bed for a two-stage heating reaction; S3, gas-solid separation, the gas is washed and dried to obtain sulfuryl fluoride.

[0011] In some embodiments of the present invention, in step S1 , the power of the plasma treatment is 100-200 W, the treatment time is 10-30 min, and the introduction rate of carbon tetrafluoride is 20-50 sccm.

[0012] In some embodiments of the present invention, the hydrogen fluoride-amine complex is a molecular sieve-supported hydrogen fluoride organic amine complex, which is prepared as follows: Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, and dry under vacuum. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution; The impregnation liquid is added dropwise to the molecular sieve, dispersed by ultrasonication, distilled under reduced pressure, and dried to obtain the hydrogen fluoride-amine complex.

[0013] In some embodiments of the present invention, the mass fraction of the impregnation liquid is 20-30%. In some embodiments of the present invention, the mass ratio of the molecular sieve to the impregnation liquid is 3:1, and the temperature of the impregnation treatment is 0-5°C.

[0014] In some embodiments of the present invention, the molecular sieve is 4A or 5A molecular sieve with a pore size of 0.4-0.5 nm.

[0015] In some embodiments of the present invention, the power of the ultrasonic dispersion is 10-20 KHz, and the dispersion time is 10-20 min.

[0016] In some embodiments of the present invention, in step S2, the temperature of the primary heating is 180-200°C; the temperature of the secondary heating is 250-350°C.

[0017] Compared with the prior art, the present invention has the following beneficial effects: This invention uses sulfuryl chloride and a hydrogen fluoride-amine complex as raw materials, combined with plasma and a fluidized bed, to improve the synthesis efficiency of sulfuryl fluoride, reduce the occurrence of side reactions, and enhance product purity. The fluidized bed design enables continuous feed of raw materials and continuous output of product, increasing production capacity by 30-40% compared to a fixed bed.

[0018] Using carbon tetrafluoride as the working gas and plasma pretreatment of the hydrogen fluoride-amine complex can construct C-F bonds on the surface of the hydrogen fluoride-amine complex, thereby increasing the reactivity of fluorine atoms and reducing the occurrence of side reactions; at the same time, the formed micro-nano rough structure increases the contact area of ​​the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying any creative work.

[0020] Figure 1 is a gas chromatogram of disulfuryl fluoride according to an embodiment of the present invention; Figure 2 It is the gas chromatogram of disulfuryl fluoride of comparative example of the present invention. DETAILED DESCRIPTION

[0021] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be purchased commercially.

[0022] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments of the present invention can be combined with each other. The present invention will be described in detail below with reference to specific embodiments.

[0023] The embodiment of the present invention provides a method for continuously preparing sulfuryl fluoride in a fluidized bed, comprising the following steps: S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex, and set aside; the plasma treatment power is 100-200 W, the treatment time is 10-30 minutes, and the carbon tetrafluoride introduction rate is 20-50 sccm; S2, preheating the fluidized bed to 150-180°C, adding the fluoride salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, and heating to 190-200°C; preheating the vaporized sulfuryl chloride to 100-120°C, and then introducing it into the fluidized bed for a two-stage heating reaction; the temperature of the first heating stage is 180-200°C; the temperature of the second heating stage is 250-350°C.

[0024] In a fluidized bed, a hydrogen fluoride-amine complex (DIPEA·3HF) reacts with vaporized sulfuryl chloride (SO₂Cl₂) at 250-350°C in a gas-solid reaction: SO₂Cl₂ + 2[R₃N·HF] → SO₂F₂ + 2[R₃N·HCl]. The chlorine atoms in the sulfuryl chloride are replaced by fluorine atoms to form sulfuryl fluoride (SO₂F₂), with the organic amine hydrochloride as a by-product. A secondary heating temperature (250-350°C) accelerates the fluorine substitution rate and increases the conversion rate to >90%. Fluoride salts provide a supplemental fluorine source for the reaction, improving the overall conversion of sulfuryl chloride.

[0025] S3, gas-solid separation, the gas is washed and dried to obtain sulfuryl fluoride.

[0026] The hydrogen fluoride-amine complex was prepared as follows: Mix the activated molecular sieve with anhydrous toluene, condense and reflux for 12 hours, and vacuum dry. The molecular sieve is 4A or 5A molecular sieve with a pore size of 0.4-0.5 nm. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 20-30%; The impregnation solution is added dropwise to the molecular sieve, ultrasonically dispersed, distilled under reduced pressure, and dried to obtain a hydrogen fluoride-amine complex. The ultrasonic dispersion power is 10-20 kHz, and the dispersion time is 10-20 minutes. The mass ratio of the molecular sieve to the impregnation solution is 3:1, and the impregnation temperature is 0-5°C.

[0027] Diisopropylethylamine trihydrofluoride is loaded on a molecular sieve by an impregnation method. The porous structure of the molecular sieve can increase the contact area between sulfuryl chloride and diisopropylethylamine trihydrofluoride, thereby improving the reaction efficiency and reducing the generation of by-products.

[0028] In an embodiment of the present invention, the fluoride salt is one or more of sodium fluoride, potassium fluoride, and barium fluoride.

[0029] The features and performance of the present invention are further described in detail below with reference to the embodiments.

[0030] Example 1 Sulfuryl fluoride was synthesized as follows: 1. Preparation of hydrogen fluoride-amine complex Select 5A molecular sieve (pore size 0.5 nm) and calcine at 550°C for 6 hours to remove adsorbed water and impurities to obtain an activated molecular sieve. Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, separate by centrifugation, and dry in a vacuum at 110°C. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 30%; The impregnation solution was added dropwise to the molecular sieve at a mass ratio of 3:1, and ultrasonic dispersion was performed for 10 minutes at a power of 10 kHz. The impregnation system was then transferred to a rotary evaporator, and the solvent was removed by reduced pressure distillation at 40°C. The system was then dried in a vacuum oven at 60°C for 12 hours to obtain a hydrogen fluoride-amine complex.

[0031] 2. Synthesis of sulfuryl fluoride in a fluidized bed S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for standby use; wherein the plasma treatment power is 100 W, the treatment time is 30 minutes, and the carbon tetrafluoride introduction rate is 20 seem; S2, preheating the fluidized bed to 150°C, adding the barium fluoride powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed via a carrier gas (helium), and heating to 190°C; preheating the vaporized sulfuryl chloride to 100°C, and introducing it into the fluidized bed at a rate of 7 g / min, to carry out a two-stage heating reaction; the temperature of the first heating stage is 200°C; the temperature of the second heating stage is 250°C; wherein, the flow rate of the carrier gas helium is 3.5 L / min, and the barium fluoride powder and the pretreated hydrogen fluoride-amine complex are introduced into the fluidized bed reactor at a rate of 17 g / min.

[0032] S3, gas-solid separation (cyclone separation), the gas is washed and dried (dried with calcium chloride) to obtain sulfuryl fluoride.

[0033] Example 2 Sulfuryl fluoride was synthesized as follows: 1. Preparation of hydrogen fluoride-amine complex Select 5A molecular sieve (pore size 0.5 nm) and calcine at 550°C for 4 hours to remove adsorbed water and impurities to obtain an activated molecular sieve. Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, separate by centrifugation, and dry in a vacuum at 110°C. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 20%; The impregnation solution was added dropwise to the molecular sieve at a mass ratio of 3:1, and ultrasonic dispersion was performed for 10 minutes at a power of 20 kHz. The impregnation system was then transferred to a rotary evaporator, and the solvent was removed by reduced pressure distillation at 40°C. The system was then dried in a vacuum oven at 60°C for 12 hours to obtain a hydrogen fluoride-amine complex.

[0034] 2. Synthesis of sulfuryl fluoride in a fluidized bed S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for standby use; wherein the plasma treatment power is 200 W, the treatment time is 10 minutes, and the carbon tetrafluoride introduction rate is 50 seem; S2, preheating the fluidized bed to 150°C, adding potassium fluoride powder and pretreated hydrogen fluoride-amine complex to the fluidized bed via a carrier gas (helium), and heating to 190°C; preheating the vaporized sulfuryl chloride to 100°C and introducing it into the fluidized bed at a rate of 7 g / min, performing a two-stage heating reaction; the primary heating temperature is 200°C; the secondary heating temperature is 350°C; the carrier gas helium flow rate is 3.5 L / min, and the potassium fluoride powder and pretreated hydrogen fluoride-amine complex are introduced into the fluidized bed reactor at a rate of 17 g / min; S3, gas-solid separation (cyclone separation), the gas is washed and dried (dried with calcium chloride) to obtain sulfuryl fluoride.

[0035] Example 3 Sulfuryl fluoride was synthesized as follows: 1. Preparation of hydrogen fluoride-amine complex Select 5A molecular sieve (pore size 0.5 nm) and calcine at 550°C for 6 hours to remove adsorbed water and impurities to obtain an activated molecular sieve. Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, separate by centrifugation, and dry in a vacuum at 110°C. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 25%; The impregnation solution was added dropwise to the molecular sieve at a mass ratio of 3:1, and ultrasonic dispersion was performed for 20 minutes at a power of 10 kHz. The impregnation system was then transferred to a rotary evaporator, and the solvent was removed by reduced pressure distillation at 40°C. The system was then dried in a vacuum oven at 60°C for 12 hours to obtain a hydrogen fluoride-amine complex.

[0036] 2. Synthesis of sulfuryl fluoride in a fluidized bed S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for standby use; wherein the plasma treatment power is 100 W, the treatment time is 30 minutes, and the carbon tetrafluoride introduction rate is 50 seem; S2, preheat the fluidized bed to 150°C, add calcium fluoride powder and pretreated hydrogen fluoride-amine complex into the fluidized bed via carrier gas (helium), and heat to 190°C; preheat the vaporized sulfuryl chloride to 100°C and introduce it into the fluidized bed at a rate of 7 g / min to carry out a two-stage heating reaction; the temperature of the first heating stage is 180°C; the temperature of the second heating stage is 250°C; the flow rate of the carrier gas helium is 3.5 L / min, and the calcium fluoride powder and pretreated hydrogen fluoride-amine complex are introduced into the fluidized bed reactor at a rate of 17 g / min.

[0037] S3, gas-solid separation (cyclone separation), the gas is washed and dried (dried with calcium chloride) to obtain sulfuryl fluoride.

[0038] Example 4 Sulfuryl fluoride was synthesized as follows: 1. Preparation of hydrogen fluoride-amine complex Select 5A molecular sieve (pore size 0.5 nm) and calcine at 550°C for 6 hours to remove adsorbed water and impurities to obtain an activated molecular sieve. Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, separate by centrifugation, and dry in a vacuum at 110°C. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 20%; The impregnation solution was added dropwise to the molecular sieve at a mass ratio of 3:1, and ultrasonic dispersion was performed for 20 minutes at a power of 10 kHz. The impregnation system was then transferred to a rotary evaporator, and the solvent was removed by reduced pressure distillation at 40°C. The system was then dried in a vacuum oven at 60°C for 12 hours to obtain a hydrogen fluoride-amine complex.

[0039] 2. Synthesis of sulfuryl fluoride in a fluidized bed S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for standby use; wherein the plasma treatment power is 200 W, the treatment time is 20 minutes, and the carbon tetrafluoride introduction rate is 50 seem; S2, preheat the fluidized bed to 180°C, add calcium fluoride powder and pretreated hydrogen fluoride-amine complex into the fluidized bed via carrier gas (helium), and heat to 190°C; preheat the vaporized sulfuryl chloride to 100°C and introduce it into the fluidized bed at a rate of 7g / min to carry out a two-stage heating reaction; the temperature of the first heating stage is 180°C; the temperature of the second heating stage is 250°C; the flow rate of the carrier gas helium is 3.5L / min, and the potassium fluoride powder and pretreated hydrogen fluoride-amine complex are introduced into the fluidized bed reactor at a rate of 17g / min.

[0040] S3, gas-solid separation (cyclone separation), the gas is washed and dried (dried with calcium chloride) to obtain sulfuryl fluoride.

[0041] Example 5 Sulfuryl fluoride was synthesized as follows: 1. Preparation of hydrogen fluoride-amine complex Select 5A molecular sieve (pore size 0.5 nm) and calcine at 550°C for 6 hours to remove adsorbed water and impurities to obtain an activated molecular sieve. Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, separate by centrifugation, and dry in a vacuum at 110°C. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution with a mass fraction of 30%; The impregnation solution was added dropwise to the molecular sieve at a mass ratio of 3:1, and ultrasonic dispersion was performed for 20 minutes at a power of 10 kHz. The impregnation system was then transferred to a rotary evaporator, and the solvent was removed by reduced pressure distillation at 40°C. The system was then dried in a vacuum oven at 60°C for 12 hours to obtain a hydrogen fluoride-amine complex.

[0042] 2. Synthesis of sulfuryl fluoride in a fluidized bed S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for standby use; wherein the plasma treatment power is 200 W, the treatment time is 10 minutes, and the carbon tetrafluoride introduction rate is 20 seem; S2, preheat the fluidized bed to 180°C, add calcium fluoride powder and pretreated hydrogen fluoride-amine complex into the fluidized bed via carrier gas (helium), and heat to 200°C; preheat the vaporized sulfuryl chloride to 100°C and introduce it into the fluidized bed at a rate of 7 g / min to carry out a two-stage heating reaction; the temperature of the first heating stage is 180°C; the temperature of the second heating stage is 250°C; the flow rate of the carrier gas helium is 3.5 L / min, and the calcium fluoride powder and pretreated hydrogen fluoride-amine complex are introduced into the fluidized bed reactor at a rate of 17 g / min.

[0043] S3, gas-solid separation (cyclone separation), the gas is washed and dried (dried with calcium chloride) to obtain sulfuryl fluoride.

[0044] Comparative Example 1 The difference from the first embodiment is that plasma treatment is not performed in step S1, and the remaining steps and raw materials are the same as those in the first embodiment.

[0045] Comparative Example 2 The difference from Example 1 is that diisopropylethylamine hydrogen fluoride complex is directly added in step S1 without molecular sieve loading, and the remaining steps and raw materials are the same as those of Example 1.

[0046] Comparative Example 3 According to the method of Example 1 of patent CN117142436A, the fluidized bed reactor is preheated to 180°C in advance, the sulfonyl chloride is preheated to 120°C, and then the carrier gas nitrogen flow rate is adjusted to 3.5L / min. Potassium bifluoride is fed into the fluidized bed reactor from the top of the fluidized bed along with the carrier gas at a speed of 17g / min by a solid feed pump, and sulfonyl chloride is fed into the fluidized bed reactor from the bottom of the fluidized bed by a liquid feed pump at a rate of 6.9g / min. The liquid feeder is first opened, and then the solid feeder is opened again. Then, the solid material and the liquid material are respectively and simultaneously fed into the fluidized bed reactor. The product generated by the reaction is sequentially passed through a gas-solid separation device (cyclone separator) and a gas separation device (gas cryogenic separator). The gas phase obtained is scrubbed and dried on a calcium chloride packed column to obtain sulfuryl fluoride.

[0047] It should be noted that the 5A molecular sieve used in the above examples and comparative examples is the HTMS-5A spherical molecular sieve produced by Liaoning Haitai Technology Development Company, and its pore size is 0.5 nm.

[0048] Experimental example The purity of sulfuryl fluoride of Examples 1 to 3 and Comparative Examples 1 to 3 was determined by gas chromatography. The results are shown in Table 1 and Table 2. Figure 1 and Figure 2 shown.

[0049] Table 1

[0050] As can be seen from the data in Table 1, the purity of the sulfuryl fluoride obtained by the preparation methods of Examples 1 to 5 is relatively high; in Comparative Example 1, the diisopropylethylamine hydrogen fluoride complex was not subjected to plasma treatment, and no C-F bond was formed on its surface. The number of active fluorine atoms was small, and by-products were easily produced, which reduced the purity of the product; in Comparative Example 2, no molecular sieve carrier was used. In the fluidized bed, the contact area between the gaseous sulfuryl chloride and the diisopropylethylamine hydrogen fluoride complex was smaller than that of Example 1, and the reaction efficiency was reduced, and by-products were more easily generated, and the product purity was also correspondingly reduced.

[0051] In summary, the present invention 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 occurrence 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.

[0052] Using carbon tetrafluoride as the working gas and plasma pretreatment of the hydrogen fluoride-amine complex can construct C-F bonds on the surface of the hydrogen fluoride-amine complex, thereby increasing the reactivity of fluorine atoms and reducing the occurrence of side reactions; at the same time, the formed micro-nano rough structure increases the contact area of ​​the reaction.

[0053] The embodiments described above are some, but not all, of the embodiments of the present invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but rather merely represents selected embodiments of the present invention. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are also within the scope of protection of the present invention.

Claims

1. A method for continuously preparing sulfuryl fluoride in a fluidized bed, characterized in that: The following steps are involved: S1, using carbon tetrafluoride as the working gas, using plasma to pre-treat the hydrogen fluoride-amine complex for use; S2, preheating the fluidized bed to 150-180°C, adding the fluoride salt powder and the pretreated hydrogen fluoride-amine complex into the fluidized bed, and heating to 190-200°C; preheating the vaporized sulfuryl chloride to 100-120°C, and then introducing it into the fluidized bed for a two-stage heating reaction; S3, gas-solid separation, the gas is washed and dried to obtain sulfuryl fluoride.

2. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 1, wherein In step S1 , the power of the plasma treatment is 100-200 W, the treatment time is 10-30 min, and the introduction rate of carbon tetrafluoride is 20-50 sccm.

3. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 1, wherein The hydrogen fluoride-amine complex is a molecular sieve-supported hydrogen fluoride organic amine complex, which is prepared as follows: Mix the activated molecular sieve with anhydrous toluene, reflux under condensation for 12 hours, and dry under vacuum. Dissolve diisopropylethylamine trihydrofluoride in anhydrous toluene to obtain an impregnation solution; The impregnation liquid is added dropwise to the molecular sieve, dispersed by ultrasonication, distilled under reduced pressure, and dried to obtain the hydrogen fluoride-amine complex.

4. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 3, wherein The mass fraction of the impregnation liquid is 20-30%.

5. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 3, characterized in that: The mass ratio of the molecular sieve to the impregnation liquid is 3:1, and the impregnation temperature is 0-5°C.

6. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 3, characterized in that: The molecular sieve is 4A or 5A molecular sieve with a pore size of 0.4-0.5 nm.

7. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 3, characterized in that: The power of the ultrasonic dispersion is 10-20 KHz, and the dispersion time is 10-20 min.

8. The method for continuously preparing sulfuryl fluoride in a fluidized bed according to claim 1, wherein In step S2, the temperature of the first heating is 180-200°C; the temperature of the second heating is 250-350°C.

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