CN108128758B

CN108128758B - SOF2And SOF4Gas preparation method and system

Info

Publication number: CN108128758B
Application number: CN201711386085.1A
Authority: CN
Inventors: 董佳家; 柯森; 李苏华
Original assignee: Shanghai Institute of Organic Chemistry of CAS
Current assignee: Zhonghongxin Investment Holding Shenzhen Co ltd
Priority date: 2017-12-20
Filing date: 2017-12-20
Publication date: 2019-12-31
Anticipated expiration: 2037-12-20
Also published as: CN108128758A

Abstract

The invention relates to the technical field of industrial chemical production and discloses a SOF (soluble organic fertilizer)₂Gas and SOF₄Method for preparing gas, system thereof, and SOF₄The gas preparation system comprises SOF₂Gas inlet pipe and fluorine gas pipeRoad, SOF₄A reaction kettle and a temperature control device; the SOF₄The preparation method of the gas comprises the following steps: step 1: mixing SOF₂Gas introduction into SOF₄In a reaction kettle; step 2: at low temperature, the SOF₄Introducing a proper amount of fluorine gas into the reaction kettle; and step 3: the SOF₄Heating the reaction kettle to room temperature and reacting for a certain time to obtain the SOF₄A gas; wherein the order of step 1 and step 2 may be interchanged. The beneficial effects of the implementation of the invention are mainly as follows: firstly provides a method for preparing high-purity SOF with low cost and easy mass production₄The preparation method and the system of the gas can realize room temperature kettle type kilogram-level SOF₄The gas phase purity of the product can reach 99.5 percent by the preparation of the gas.

Description

SOF2And SOF4Gas preparation method and system

Technical Field

The invention relates to the technical field of industrial chemical production, in particular to a SOF (soluble organic fertilizer)₂Gas and sulfur oxide tetrafluoride (SOF)₄) A method and system for preparing gas.

Background

As known to those skilled in the art, tetrafluorooxysulfide (SOF)₄) It is a colorless, pungent gas at room temperature. SOF₄Has wide potential research value and good application prospect in biochemistry, medicine preparation and polymer materials (S.Li, P.Wu, J.E.Moses, K.B.Sharpless, Angew. chem.int.Ed.2017,56,2903-₄Has very important significance.

However, SOF₄The preparation method is few, and only very early foreign documents can be used as reference, and the preparation method can be only theoretically prepared or can be only prepared on a small scale.

Theoretically, SOF₄Can be prepared from SO₃F₂React with iodine anions in aqueous solution, however f.b. Dudley et al (f.b. Dudley, g.h.cady, d.f. eggers, jr.j.am.chem.soc. 1956,78,290) actually produce only SOF₄ ^-Ion, no practical preparation of SOF₄And (5) producing the product. Also w.c. smith et al (w.c. smith, v.a. engelhardt,j.am.chem.soc.1960, 82,3838) use expensive, highly corrosive, highly toxic, not readily available SF₄And NO₂Preparation of SOF as raw material₄However, this production method needs to be carried out under high temperature conditions, and the gaseous raw material generates extremely high pressure and extremely high corrosiveness under high temperature conditions. For example: SF₄And NO₂When the reaction is heated to 230 ℃, the pressure generated in the reaction process is up to 11.7 MPa. The high pressure and the strong corrosiveness of the raw materials in the reaction process have extremely high requirements on the reaction equipment, so that the method cannot be applied to the SOF₄The scale-up production of (1).

Furthermore, W.KWasoik and H.Jonas.Z et al (W.KWasoik, "organic Chemistry," 1948, Vol.I, pp.192-193; H.Jonas.Z.anorg.allgem.chem.,1951, 265,273) apply SOF₂And fluorine gas to 150 ℃, and then producing SOF by using expensive metal platinum (Pt) net as catalyst₄. However, this process requires an ultra-low temperature (-198 ℃) during operation and produces SOFs₄Has low purity (only 60%) and contains large amount of SF₆And SO₂F₂The preparation amount is only about ten grams at a time. The metal catalysts utilized in this process are expensive and not easily handled at ultra-low temperatures, which is detrimental to SOF₄The scale-up production of (1).

In summary, the current preparation of SOFs₄The method has the defects of harsh reaction conditions, expensive and not easily obtained reaction raw materials, use of expensive metal catalysts and preparation of the SOF₄The low purity and low throughput limit further scale-up of these processes. Moreover, these processes are harsh in reaction conditions and the strong corrosiveness of the starting materials also place extreme demands on the reaction equipment, which all add to the preparation of SOF₄The cost of (a).

Disclosure of Invention

The invention aims to solve the technical problem of the prior preparation of SOF₄The gas method has the defects of harsh reaction conditions, expensive and unavailable reaction raw materials and SOF (soluble organic silicon) prepared by the method₄The low purity of the gas and the low throughput limit further scale-up.

To understandIn order to solve the technical problem, the invention discloses a SOF₄The preparation method and the system of the gas can realize room temperature kettle type kilogram-level SOF₄The technical scheme of the invention is implemented as follows:

SOF₄A method for producing a gas, comprising the steps of: step 1: mixing SOF₂Gas introduction into SOF₄In a reaction kettle; step 2: at low temperature, the SOF₄Introducing a proper amount of fluorine gas into the reaction kettle; and step 3: the SOF₄Heating the reaction kettle to room temperature to obtain SOF₄A gas; wherein the order of step 1 and step 2 may be interchanged.

Preferably, the method further comprises the step of pretreating the SOF₄Vacuumizing the reaction kettle; the SOF₂The gas is SOF with the purity of more than 98.0 percent₂A gas.

Preferably, in the step 2, the SOF₄Introducing fluorine gas into the reaction kettle at the low temperature of-50 to-150 ℃, wherein the low temperature is preferably-50 to-130 ℃, and more preferably-50 to-80 ℃; the SOF₂The molar ratio of the gas to the fluorine gas is 1 (0.5 to 2).

Preferably, in the step 3, the SOF₄After the temperature of the reaction kettle is raised to the room temperature, the reaction time is 10-40 hours, preferably 20-30 hours, and more preferably 30 hours; then cooling, vacuumizing, heating, and transferring to SOF₄Storage vessel to obtain SOF₄A gas.

Preferably, the system also comprises a SOF₄Further purification of the gas: SOF with the purity of 90.0-98.0 percent₄Gas transfer to SOF containing DMF₄Placing the mixture in a purification kettle for 3-20 hours, preferably 3-10 hours to obtain purified SOF₄Gas, SOF₄The purity of the gas reaches more than 99.0 percent.

SOF₂A method for producing a gas, comprising the steps of: step 1-1: evenly mixing a fluorinating reagent, thionyl chloride and a solvent, adding the mixture into SOF₂Heating, refluxing and stirring in a reaction kettle to prepare SOF₂Gas, wherein the temperature of the condenser pipe is controlled between-20 ℃ and-50 ℃, andobtaining SOF₂A gas; step 1-2: subjecting the SOF to₂Gas transfer to SOF₂In a purification kettle, obtaining purified SOF after adsorption reaction for a certain time₂A gas.

Preferably, in the step 1-1, the molar ratio of the fluorinating agent to the thionyl chloride to the solvent is 6:0.838: 5.5; the temperature of the condenser pipe is controlled to be-35 ℃ to-50 ℃, and is preferably controlled to be-35 ℃ to-40 ℃.

Preferably, in the step 1-1, the fluorinating agent is sodium fluoride, potassium fluoride, cesium fluoride or hydrofluoric acid; the solvent is acetonitrile.

Preferably, in the step 1-2, anhydrous KF is added for adsorption reaction, and after the adsorption reaction is carried out for a certain time, the SOF with the purity of more than 98.0 percent is obtained₂And gas, wherein the adsorption reaction time is 2-30 days, preferably 2-20 days, and more preferably 2-10 days.

Preferably, the method further comprises the following steps 1-3: when KF color does not turn yellow, adsorbed SOF is₂SOF to which gas is transferred₂And storing the mixture in a kettle for later use.

Preferably, a SOF₄The gas preparation system comprises SOF₂Gas inlet duct, fluorine gas duct, SOF₄A reaction kettle and a temperature control device; the SOF₂Gas inlet duct and said fluorine gas duct and said SOF₄The reaction kettle is connected, the SOF₄The reaction kettle is arranged in the temperature control device.

Preferably, the SOF₄The gas preparation system also comprises a vacuum emptying pipeline and a SOF₄Purification kettle, vacuum evacuation pipeline and SOF₄The reaction kettle is connected, the SOF₄Reaction kettle and SOF₄Purification kettle connection, said SOF₄Purification kettle and SOF₄The storage kettle is connected.

Preferably, the SOF₄The gas preparation system further comprises a SOF₂Gas preparation apparatus, said SOF₂The gas preparation plant comprises a SOF₂Reaction kettle, heating water bath circulating pump, low-temperature circulating pump, constant-pressure dropping funnel, condensing device and SOF₂Purification kettle and SOF₂Storing the kettle; wherein the SOF₂The reaction kettle is connected with the condensing device, the heating water bath circulating pump and the constant-pressure dropping funnel; the condensing device is respectively connected with the low-temperature circulating pump and the SOF₂Connecting the purification kettle; the SOF₂Purification kettle and SOF₂Storage vessel connected, the SOF₂Passing the storage kettle through the SOF₂Air inlet duct and said SOF₄The reaction kettle is connected.

The beneficial effects of the implementation of the invention are mainly as follows:

1. the invention firstly provides a method for preparing high-purity SOF with low cost₄The invention has the advantages of cheap and easily obtained raw materials, simple preparation system and cyclic use.

2. The invention provides a practical SOF easy to be produced in large scale₄The gas preparation method and the system thereof have the advantages of mild reaction conditions, simple and convenient production process and high purity of the prepared product. The gas phase purity of the primary crude product can reach 98.0 percent, and a hectogram-scale product can be generated at one time. The gas phase purity of the purified product can reach 99.5%.

Drawings

For a better understanding of the technical aspects of the invention, reference is made to the following drawings, which illustrate the prior art or embodiments. These drawings will briefly illustrate some embodiments or products or methods related to the prior art. The basic information for these figures is as follows:

FIG. 1 is an example, SOF₂A schematic diagram of a gas preparation system;

in the above drawings, the reference numbers and their corresponding technical features are as follows:

1-constant pressure dropping funnel, 2-SOF₂A reaction kettle, 3-a heating water bath circulating pump, 4-a condensing device, 41-a drying tower, 42-a condensing pipe, 43-a cold well, 5-a low-temperature circulating pump, 6-SOF₂Purification kettle, 7-SOF₂Storage tank, 8-SOF₂Gas inlet line, 9-fluorine gas line, 10-vacuum evacuation line, 11-SOF₄Reaction kettle, 12-temperature control device, 13-SOF₄A purification kettle is arranged in the reaction kettle,14-SOF₄and (5) storing the kettle.

Detailed Description

Now, the technical solutions or advantages of the embodiments of the present invention will be further described, and it is obvious that the described embodiments are only some implementations of the present invention, and not all implementations. In some embodiments, as shown in FIG. 1, the present invention provides a SOF₄A system for the production of gas, the system comprising a SOF₂Gas production plant and SOF₄A gas preparation device. SOF₂Gas preparation device for raw material SOF₂Mass production and purification of gases. SOF₄Gas preparation device for product SOF₄The amplification and purification of gases.

Wherein the SOF₂The gas preparation device comprises: SOF₂A reaction kettle 2, a heating water bath circulating pump 3, a low-temperature circulating pump 5, a constant-pressure dropping funnel 1, a condensing device 4 and SOF₂Purification kettle 6 and SOF₂And a storage tank 7. Wherein the SOF₂The reaction kettle 2 is connected with the condensing device 4, the heating water bath circulating pump 3 and the constant-pressure dropping funnel 1; the condensing device 4 is connected with the low-temperature circulating pump 5; the condensing unit 4 and SOF₂The purification kettle 6 is connected; the SOF₂Purification kettle 6 and SOF₂The storage kettle 7 is connected, the SOF₂Passing the storage kettle 7 through the SOF₂Air inlet duct 8 and SOF₄The reaction kettle 11 is connected. Preferably, the SOF₂The reaction kettle 2 is SOF₂A glass reaction kettle; the volume of the constant pressure dropping funnel 1 is 1L. The condensing device 4 comprises at least five glass cooling wells 43 and at least one glass drying tower 41 which are connected in sequence. The low-temperature circulating pump 5 is connected with a condensing pipe 42 in the condensing device 4; the condensing device 4 is connected with the SOF through a rubber pipe₂The reaction kettle 2 is connected. Preferably, the number of the low-temperature circulating pumps 5 is at least 2. The heating water bath circulating pump 3 and the low temperature circulating pump 5 in this embodiment are purchased from Zhengzhou great wall science and trade company, Inc., and have a model number of DLSB-10/20. Wherein, SOF₂Purification kettle 6, SOF₂The material of the storage kettle 7 is SUS304, and the storage kettle is welded as required.

WhereinThe SOF₄The gas preparation device comprises: SOF₂Air inlet duct 8, SOF₄Reaction kettle 11, temperature control device 12, fluorine gas pipeline 9, vacuum emptying pipeline 10 and SOF₄Storage tank 14. The SOF₂Gas inlet pipe 8, fluorine gas pipe 9, vacuum evacuation pipe 10 and SOF₄The reaction kettle 11 is connected, and the SOF is₄The reaction kettle is arranged in the temperature control device 12, and the SOF₄Reaction kettle 11 and SOF₄The storage tank 14 is connected. Preferably, the SOF₄The gas preparation system further comprises a SOF₄Purification vessel 13, the SOF₄Reaction kettle 11 and SOF₄Purification kettle 13 connected, the SOF₄Purification kettle 13 and the SOF₂The storage tank 14 is connected. Preferably, the SOF₄Reaction kettle 11 and SOF₄Purification kettle 13 and SOF₄The storage kettle is an autoclave. The autoclave is made of SUS304, which is cheap and corrosion resistant. Wherein the SOF₂The air inlet duct 8 is a metal hose.

The invention provides a SOF₂The preparation method of the gas comprises the following specific steps:

step 1-1: evenly mixing a fluorinating reagent, thionyl chloride and a solvent, adding the mixture into SOF₂In the reaction kettle 2, heating, refluxing and stirring are carried out to prepare the SOF₂Solution, wherein the temperature of the condensation pipe 42 is controlled between-20 ℃ and-50 ℃, and SOF is obtained₂A gas. Preferably, the solvent is acetonitrile (CH)₃CN); the molar ratio of the fluorinating agent to the thionyl chloride to the solvent is 6:0.838: 5.5.

preferably, 50L of glass SOF₂The reaction kettle 2 is connected with a heating water bath circulating pump 3; one of the low-temperature circulating pumps 5 is connected to the condensing pipe 42 in the condensing unit 4; the condensation pipe 42 is connected with the SOF through a rubber pipe₂The reaction kettle 2 is connected. After the equipment is connected in sequence, the heating water bath circulating pump 3 is heated to 60 ℃ and circulated, so that the whole equipment system is kept to have good air tightness and the air path is smooth.

First, SOF₂Nitrogen gas was introduced into the reaction vessel 2 to discharge the air in the whole system. To SOF₂Adding a fluorinated reagent and an acetonitrile solution into the reaction kettle 2 in sequenceStirring, adding thionyl chloride solution into constant pressure dropping funnel 1, and adding to SOF₂Thionyl chloride is sequentially added dropwise into the reaction kettle 2.

Secondly, heating, refluxing and stirring to prepare SOF₂During the collection of the solution, the temperature in the condensation pipe 42 of the condensation device 4 is kept at a low temperature. The cold well 43 is placed in an ethanol solution at the temperature of minus 50 ℃ to minus 80 ℃, and the last glass cold well 43 is connected with the glass drying tower 41, so that the air path is kept smooth. The temperature of the condenser tube 42 is controlled between minus 20 ℃ and minus 50 ℃, and after a certain reaction time, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂A liquid. Preferably, the reaction time is 6 hours. Preferably, the ethanol solution is-80 ℃.

Step 1-2: SOF in the cold well 43₂Transfer of solution to SOF₂In purification vessel 6, SOF₂Anhydrous KF and anhydrous CaCl are filled in the purification kettle 6₂After standing for 1-30 days, observing the color of KF, and if the KF is yellowed, adding anhydrous KF again to continue to react with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂The autoclave was stored for future use. Preferably, the SOF₂The purification vessel 6 was a 10L autoclave. Preferably, the anhydrous KF is 500g and the anhydrous CaCl is₂The weight was 500 g.

The invention produces at least 3kg of SOF at one time₂Liquid, and vapor phase purified SOF₂The highest yield reaches 99.9 percent, and the highest yield reaches 90 percent.

The invention provides a SOF₄A method for producing a gas, comprising the steps of:

step 1: mixing SOF₄Reactor 11 passed SOF₂Air inlet duct 8 and SOF₂The storage kettle 7 is connected; SOF with gas phase purity of more than 98.0 percent₂Gas introduction into SOF₄In reaction vessel 11. Calculating the required SOF according to the room temperature at the time₂The amount of (2) is, for example, 27 ℃ and SOF is introduced into a 10L reactor₂0.638 mol. Preferably, SOF is passed₂Before, the SOF is subjected to₄Reaction kettle11, vacuumizing.

Step 2: at low temperature, the SOF₄A proper amount of fluorine gas is introduced into the reaction kettle 11, wherein the SOF₂The molar ratio of the gas to the fluorine gas is 1mol (0.5 to 2 mol). Introducing SOF₂SOF of₄The reaction kettle 11 is put into a temperature control device 12 for cooling, and the temperature in the reaction kettle is detected at the same time. When the temperature reaches-50 ℃ to-150 ℃, a copper pipe is used for connecting the fluorine gas pipeline 9 and the SOF₄And (3) opening a fluorine gas valve of the reaction kettle 11, so that fluorine gas slowly enters the reaction kettle, and pumping away air in the pipeline while introducing the fluorine gas. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction kettle 11 is reduced by about 11 ℃ to 15 ℃. Preferably, temperature control device 12 is a solution of liquid nitrogen/ethanol. Wherein the order of step 1 and step 2 may be interchanged.

And step 3: SOF₄The reaction kettle 11 is slowly heated up to room temperature and is placed for 10 to 40 hours at the room temperature. SO in the process_F4The pressure of the reaction tank 11 is continuously decreased. SOF after 30 hours₄The pressure in the reaction tank 11 continues to decrease, but the rate of decrease is slow. Then adding SOF₄The reaction kettle 11 is placed in a temperature control device 12 for cooling, and when the temperature is reduced to a certain temperature, redundant fluorine gas is discharged through a vacuum discharge pipeline 10. Specifically, a grab vacuum pump is used to pump off excess fluorine gas and to try to vacuum, the lower the pump, the lower the final oxygen/nitrogen content. All products in the reaction kettle are transferred to the SOF₄Storage tank 14 from which SOF is obtained₄The yield of the gas is more than 70%, and the gas phase purity is more than 90.0%. Preferably, temperature control device 12 is a solution of liquid nitrogen/ethanol.

And 4, step 4: SOF₄Further purifying the gas, namely, using SOF with gas phase purity of 90.0-98.0 percent₄Gas transfer to SOF containing Dimethylformamide (DMF)₄Standing in a purification kettle 13 for reaction for a certain time, SOF₄The purity of the gas phase reaches 99.3 to 99.7 percent.

The present invention uses a cheap and safe industrial purity fluorinating agent, fluoride salts such as sodium fluoride, potassium fluoride, cesium fluoride, hydrofluoric acid (NaF, KF, CsF, HF) and thionyl chloride (SOCl)₂) And acetonitrileTaking SOF₂As raw material, and then SOF₂Fluorine gas is introduced at low temperature, then the temperature is raised to room temperature, and SOF₂And reacting fluorine gas at room temperature to obtain SOF₄。

The invention proves that the product can be stably produced after 10 times of factory runs, the gas phase purity of the primary crude product can reach 98.0 percent, and the product with hectogram scale can be produced once. And this produces SOF₄The method of (3) is a very practical and easily scalable method. The present invention does not utilize any expensive metal catalyst, nor does it heat. The reaction kettle is made of common steel and can be recycled for multiple times. The preparation method has incomparable advantages measured from the aspects of reaction raw materials, reaction conditions, reaction safety, production cost and yield.

Example 1

The present embodiment provides a SOF₂A method for preparing gas.

Step 1-1: first, SOF₂And introducing nitrogen into the reaction kettle 2 for 30min, and discharging the air in the whole system. To 50L glass SOF₂15kg of sodium fluoride and 12kg of acetonitrile solution are sequentially added into a reaction kettle 2 and uniformly stirred, 5.5kg of thionyl chloride solution is added into a constant-pressure dropping funnel 1, and thionyl chloride is sequentially dropped into the reaction kettle for 3 hours.

Secondly, heating, refluxing and stirring to prepare SOF₂In the process of collecting the solution, the temperature in the condenser tube 42 is always kept between minus 35 ℃ and minus 40 ℃, and after 6 hours of reaction, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 87%.

Step 1-2: SOF in the cold well 43₂Solution converterMove to 10L SOF₂In purification kettle 6. SOF₂After the purification kettle 6 is placed for 2 days, the color of KF is observed, if the KF has become yellow, anhydrous KF is added again to continue to react with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for later use and purified SOF₂Reaching 99.9 percent.

Example 2

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

step 1-1: first, SOF₂And introducing nitrogen into the reaction kettle 2 for 30min, and discharging the air in the whole system. To SOF₂20.7kg of potassium fluoride and 12kg of acetonitrile solution are sequentially added into a reaction kettle 2 and uniformly stirred, 5.5kg of thionyl chloride solution is added into a constant-pressure dropping funnel 1, and thionyl chloride is sequentially dropped into the reaction kettle for 3 hours.

Heating reflux stirring for preparing SOF₂In the process of collecting the solution, the temperature in the condenser tube 42 is always kept between minus 35 ℃ and minus 40 ℃, and after 6 hours of reaction, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 88%.

Step 1-2: SOF in the cold well 43₂The solution was rapidly transferred to 10L SOF₂In purification kettle 6. SOF₂After the purification kettle 6 is left for 2 days, the color of KF is observed, and if a large amount of yellowing occurs, anhydrous KF is added again to continue to react with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for use, purified SOF₂Reaching 99.9 percent.

Example 3

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

step 1-1: first, SOF₂And introducing nitrogen into the reaction kettle 2 for 30min, and discharging the air in the whole system. To SOF₂53.97kg of cesium fluoride and 12kg of acetonitrile solution are sequentially added into a reaction kettle 2 and uniformly stirred, 5.5kg of thionyl chloride solution is added into a constant-pressure dropping funnel 1, and thionyl chloride is sequentially dropped into the reaction kettle, wherein the dropping time is 3 hours.

Heating reflux stirring for preparing SOF₂In the process of collecting the solution, the temperature in the condenser tube 42 is always kept between minus 35 ℃ and minus 40 ℃, and after 6 hours of reaction, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 87%.

Example 4

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

step 1-1: first, SOF₂And introducing nitrogen into the reaction kettle 2 for 30min, and discharging the air in the whole system. To SOF₂53.97kg of hydrofluoric acid and 12kg of acetonitrile solution are sequentially added into a reaction kettle 2 and uniformly stirred, 5.5kg of thionyl chloride solution is added into a constant-pressure dropping funnel 1, and thionyl chloride is sequentially dropped into the reaction kettle for 3 hours.

Heating reflux stirring for preparing SOF₂In the collecting process of the solution, the temperature in the condenser tube 42 is always kept between minus 35 ℃ and minus 40 ℃, and after 6 hours of reaction, a solution can be collected in the glass cooling well 43The colorless and transparent solution is SOF₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 89%.

Example 5

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

step 1-1: first, SOF₂And introducing nitrogen into the reaction kettle 2 for 30min, and discharging the air in the whole system. To SOF₂15kg of sodium fluoride and 12kg of acetonitrile solution are sequentially added into a reaction kettle 2 and uniformly stirred, 5.5kg of thionyl chloride solution is added into a constant-pressure dropping funnel 1, and thionyl chloride is sequentially dropped into the reaction kettle for 3 hours.

Heating reflux stirring for preparing SOF₂In the process of collecting the solution, the temperature in the condenser tube 42 is always kept between minus 20 ℃ and minus 30 ℃, and after 6 hours of reaction, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 90%.

Step 1-2: SOF in the cold well 43₂The solution was rapidly transferred to 10L SOF₂In purification tank 66. SOF₂After the purification kettle 6 is left for 2 days, the color of KF is observed, and if a large amount of yellowing occurs, anhydrous KF is added again to continue to react with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for use, purified SOF₂Reaching 98.0 percent.

Example 6

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

Heating reflux stirring for preparing SOF₂In the process of collecting the solution, the temperature in the condenser tube 42 is always kept between-40 ℃ and-50 ℃, and after 6 hours of reaction, a colorless and transparent solution which is SOF can be collected in the glass cold well 43₂Liquid, producing at least 3kg of SOF at a time₂Liquid, yield 86%.

Example 7

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

Step 1-2: SOF in the cold well 43₂The solution was rapidly transferred to 10L SOF₂In purification kettle 6. SOF₂After the purification vessel 6 was left for 10 days, the color of KF was observed, and if there was a large amount of yellowing, anhydrous KF was added again to continue with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for use, purified SOF₂Reaching 99.9 percent.

Example 8

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

Step 1-2: SOF in the cold well 43₂The solution was rapidly transferred to 10L SOF₂In purification kettle 6. SOF₂After the purification kettle 6 is left for 20 days, the color of KF is observed, and if there is a large amount of yellowing, anhydrous KF is added again to continue to react with SOF₂Placing the components together; if notYellowing to obtain purified SOF₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for use, purified SOF₂Reaching 99.0 percent.

Example 9

The present embodiment provides a SOF₂A method for preparing gas.

The present embodiment differs from embodiment 1 in that:

Step 1-2: SOF in the cold well 43₂The solution was rapidly transferred to 10L SOF₂In purification kettle 6. SOF₂After the purification kettle 6 is left for 30 days, the color of KF is observed, if a large amount of yellowing occurs, anhydrous KF is added again to continue to react with SOF₂Placing the components together; if there is no yellowing, a purified SOF is obtained₂Gas, and adsorbing the adsorbed purified SOF₂Gas transfer to a clean SOF₂Storage tank 7 for use, purified SOF₂Reaching 99.0 percent.

Example 10

The present embodiment provides a SOF₄A method for preparing gas.

Step 1: 0.638mol of SOF with a gas phase purity of 98.0% or more₂Gas is introduced into the SOF through a metal hose₄In reaction vessel 11.

Step 2: introducing SOF₂SOF of₄Liquid nitrogen is put into the reaction kettle 11Cooling in ethanol solution and detecting SOF₄The temperature in the reaction vessel 11. When the temperature reaches-100 ℃, a copper pipe is used for connecting the fluorine gas pipeline 9 with the SOF₄The reaction vessel 11 was opened with a fluorine gas valve to let 0.319mol of fluorine gas slowly enter the SOF₄In the reaction vessel 11, fluorine gas was introduced and air in the piping was evacuated. The fluorine gas valve is closed, and the temperature of the reaction kettle is reduced by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 73%, gas phase purity 90.0%.

Example 11

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-50 ℃, a fluorine gas valve is opened, 0.319mol of fluorine gas slowly enters the reaction kettle, and air in the pipeline is pumped away while the fluorine gas is introduced. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄Reaction ofThe kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 70%, gas phase purity 90.0%.

Example 12

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-80 ℃, a fluorine gas valve is opened, 0.319mol of fluorine gas slowly enters the reaction kettle, and air in the pipeline is pumped away while the fluorine gas is introduced. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 72%, gas phase purity 90.0%.

Example 13

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-130 ℃, a fluorine gas valve is opened to allow 0.319mol of fluorine gas to slowly enter the SOF₄In the reaction vessel 11, fluorine gas was introduced and air in the piping was evacuated. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 70%, gas phase purity 92.0%.

Example 14

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-150 ℃, a fluorine gas valve is opened to allow 0.319mol of fluorine gas to slowly enter the SOF₄In the reaction vessel 11, fluorine gas was introduced and air in the piping was evacuated. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours pressingThe force continues to decrease but the rate of decrease is slower. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 73%, gas phase purity 94.0%.

Example 15

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-100 ℃, a fluorine gas valve is opened to allow 0.702mol of fluorine gas to slowly enter the SOF₄In the reaction vessel 11, fluorine gas was introduced and air in the piping was evacuated. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 80%, gas phase purity 95.0%.

Example 16

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

step 1: mixing SOF₄The reaction kettle 11 is vacuumized, and 0.63 percent of vacuum is added8mol of SOF with gas phase purity of more than 98.0 percent₂Gas is introduced into the SOF through a metal hose₄In reaction vessel 11.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 85%, gas phase purity 97.0%.

Example 17

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

step 1: mixing SOF₄Vacuumizing the reaction kettle 11, and adding more than 98.0 percent of SOF with the gas phase purity of 0.638mol₂Gas is introduced into the SOF through a metal hose₄In reaction vessel 11.

Step 2: introducing SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling, and the SOF is detected simultaneously₄The temperature in the reaction vessel 11. When the temperature reaches-100 ℃, a fluorine gas valve is opened to allow 0.829mol of fluorine gas to slowly enter the SOF₄In the reaction vessel 11, fluorine gas was introduced and air in the piping was evacuated. The fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃.

And step 3: SOF₄The reaction vessel 11 was slowly warmed up to room temperature, and left at room temperature for about 30 hours. SOF in this process₄The pressure of the reaction tank 11 is continuously decreased. After 30 hours the pressure continued to decrease, but the rate of decrease slowed. Then adding SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a grab vacuum pump is used for pumping away redundant fluorine gas. SOF₄Slowly heating the reaction kettle 11 to room temperature, and heating the SOF to room temperature₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 84%, gas phase purity 98.0%.

Example 18

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

step 1: mixing 10L SOF₄The reaction kettle 11 is vacuumized as much as possible by a vacuum pump, and SOF₄The reaction kettle 11 is connected with the storage SOF through a metal hose₂The storage kettles are connected. If necessary, 0.638mol of SOF₂。

Step 2: general good SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling. When the temperature reaches-100 ℃, a copper pipe is used for connecting the fluorine gas pipeline 9 with the SOF₄Reaction vessel 11, SOF₄0.957mol of fluorine gas was fed into the reaction vessel 11.

And step 3: the fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃. SOF₄The reaction vessel 11 was slowly warmed up to room temperature. And left at room temperature for about 30 hours. In-process SOF₄The pressure of the reaction tank 11 is continuously decreased. In the process of SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a special pump is used for pumping away redundant fluorine gas. SOF₄The reaction vessel 11 was slowly warmed to room temperature and then warmed to room temperature. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 83%, gas phase purity 98.0%.

Example 19

The embodiment is providedFor providing a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: general good SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling. When the temperature reaches-100 ℃, a copper pipe is used for connecting the fluorine gas pipeline 9 with the SOF₄Reaction vessel 11, SOF₄1.276mol of fluorine gas was fed into the reaction vessel 11.

And step 3: the fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃. SOF₄The reaction vessel 11 was slowly warmed up to room temperature. And left at room temperature for about 30 hours. In-process SOF₄The pressure of the reaction tank 11 is continuously decreased. In the process of SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a special pump is used for pumping away redundant fluorine gas. SOF₄The reaction vessel 11 was slowly warmed to room temperature and then warmed to room temperature. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 82%, gas phase purity 98.0%.

Example 20

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

Step 2: general good SOF₂SOF of₄The reaction kettle 11 is put into a liquid nitrogen/ethanol solution for cooling. When the temperature reaches-100 ℃, a copper pipe is used for connecting the fluorine gas pipeline 9 with the SOF₄Reaction vessel 11, SOF₄0.702mol of fluorine gas was fed into the reaction vessel 11.

And step 3: the fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃. SOF₄The reaction vessel 11 was slowly warmed up to room temperature. And left at room temperature for about 10 hours. In-process SOF₄The pressure of the reaction tank 11 is continuously decreased. In the process of SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a special pump is used for pumping away redundant fluorine gas. SOF₄The reaction vessel 11 was slowly warmed to room temperature and then warmed to room temperature. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 80%, gas phase purity 97.0%.

Example 21

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

And step 3: the fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃. SOF₄The reaction vessel 11 was slowly warmed up to room temperature. And left at room temperature for about 20 hours. In-process SOF₄The pressure of the reaction tank 11 is continuously decreased. In the process of SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a special pump is used for pumping away redundant fluorine gas. SOF₄The reaction vessel 11 was slowly warmed to room temperature and then warmed to room temperature. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 81%, gas phase purity 97.0%.

Example 22

The present embodiment provides a SOF₄A method for preparing gas.

The present embodiment differs from embodiment 10 in that:

And step 3: the fluorine valve is turned off, at this time SOF₄The temperature of the reaction vessel 11 is lowered by about 12 ℃. SOF₄The reaction vessel 11 was slowly warmed up to room temperature. And left at room temperature for about 40 hours. In-process SOF₄The pressure of the reaction tank 11 is continuously decreased. In the process of SOF₄The reaction kettle 11 is placed in a liquid nitrogen/ethanol solution for cooling, and when the temperature is reduced to-100 ℃, a special pump is used for pumping away redundant fluorine gas. SOF₄The reaction vessel 11 was slowly warmed to room temperature and then warmed to room temperature. Mixing SOF₄The products in the reaction vessel 11 were all transferred to the SOF₄Storage tank 14 from which SOF is obtained₄Gas, yield 82%, gas phase purity 97.0%.

Example 23

This example provides a further purification process for SOF4 gas.

And 4, step 4: SOF with gas phase purity of 90.0-92.0%₄Gas transfer to SOF containing Dimethylformamide (DMF)₄Standing in a purification kettle 13 for reaction, standing at room temperature for 3 hours, and performing SOF₄The gas phase purity of (2) can reach 95.0%.

Example 24

This embodiment provides a SOF₄Further purification of the gas.

And 4, step 4: SOF with the purity of 95.0 to 98.0 percent₄Gas transfer to SOF containing Dimethylformamide (DMF)₄Standing in a purification kettle 13 for reaction, standing at room temperature for 5 hours, and performing SOF₄The purity of the gas phase can reach 99.0%.

Example 25

This embodiment provides a SOF₄Further purification of the gas.

And 4, step 4: SOF with the purity of 95.0 to 98.0 percent₄Gas transfer to SOF containing Dimethylformamide (DMF)₄Standing in a purification kettle 13 for reaction, standing at room temperature for 10 hours, and performing SOF₄The purity of the gas phase can reach 99.5 percent.

Example 26

This embodiment provides a SOF₄Further purification of the gas.

And 4, step 4: SOF with the purity of 95.0 to 98.0 percent₄Gas transfer to SOF containing Dimethylformamide (DMF)₄Standing in a purification kettle 13 for reaction, standing at room temperature for 20 hours, and performing SOF₄The gas phase purity of the product can reach 99.1 percent

Finally, it should be noted that the above-mentioned embodiments are typical and preferred embodiments of the present invention, and are only used for explaining and explaining the technical solutions of the present invention in detail, so as to facilitate the reader's understanding, and are not used to limit the protection scope or application of the present invention. Therefore, any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be covered within the protection scope of the present invention.

Claims

1. SOF₄The preparation method of the gas is characterized by comprising the following steps:

step 1: mixing SOF₂Gas introduction into SOF₄In a reaction kettle;

step 2: at low temperature, the SOF₄Introducing a proper amount of fluorine gas into the reaction kettle;

and step 3: the SOF₄Heating the reaction kettle to room temperature for reaction to obtain SOF₄A gas;

wherein the sequence of step 1 and step 2 can be interchanged;

further comprises the following pretreatment step of firstly pretreating the SOF₄Vacuumizing the reaction kettle; the SOF₂The gas is SOF with the purity of more than 98.0 percent₂A gas;

in the step 2, the SOF₄Fluorine gas is introduced into the reaction kettle at the low temperature of-50 to-150 ℃, and the SOF₂The molar ratio of the gas to the fluorine gas is 1 (0.5 to 2).

2. The SOF of claim 1₄The preparation method of the gas is characterized in that: the SOF₄Fluorine gas is introduced into the reaction kettle at the low temperature of-50 ℃ to-130 ℃.

3. The SOF of claim 1₄The preparation method of the gas is characterized in that: the SOF₄Fluorine gas is introduced into the reaction kettle at the low temperature of-50 ℃ to-80 ℃.

4. The SOF of claim 1₄The preparation method of the gas is characterized in that: in the step 3, the SOF₄The reaction time is 10-40 hours after the temperature of the reaction kettle is raised to the room temperature; then cooling, vacuumizing, heating, and transferring to the SOF₄Storage vessel to obtain SOF₄A gas.

5. The SOF of claim 4₄The preparation method of the gas is characterized in that: the SOF₄The reaction time is 20-30 hours after the temperature of the reaction kettle is raised to the room temperature.

6. The SOF of claim 4₄The preparation method of the gas is characterized in that: the SOF₄The reaction time was 30 hours after the temperature of the reaction vessel was raised to room temperature.

7. The SOF of claim 1₄The preparation method of the gas is characterized in that: further comprises a SOF₄Further purification of the gas: SOF with the purity of 90.0-98.0 percent₄Transfer of gas to a medium containing DMSaid SOF of F₄Placing the mixture in a purification kettle for 3-20 hours to obtain purified SOF₄Gas, SOF₄The purity of the gas reaches more than 99.0 percent.

8. The SOF of claim 7₄The preparation method of the gas is characterized in that: SOF with the purity of 90.0-98.0 percent₄Gas transfer to said SOF containing DMF₄And placing the mixture in a purification kettle for 3-10 hours.

9. SOF₂The preparation method of the gas is characterized by comprising the following steps:

step 1-1: evenly mixing a fluorinating reagent, thionyl chloride and a solvent, adding the mixture into SOF₂Heating, refluxing and stirring in a reaction kettle to prepare SOF₂Gas, wherein the temperature of the condensing pipe is controlled between-20 ℃ and-50 ℃, and SOF is obtained₂A gas, wherein the fluorinating agent is sodium fluoride, potassium fluoride, cesium fluoride or hydrofluoric acid;

step 1-2: subjecting the SOF to₂Gas transfer to SOF₂In a purification kettle, after adsorption reaction for a certain time, SOF with the purity of more than 98.0 percent is obtained₂A gas.

10. The SOF of claim 9₂The preparation method of the gas is characterized in that: in the step 1-1, the molar ratio of the fluorination reagent to the thionyl chloride to the solvent is 6:0.838: 5.5; the temperature of the condenser pipe is controlled to be-35 ℃ to-50 ℃.

11. The SOF of claim 10₂The preparation method of the gas is characterized in that: the temperature of the condenser pipe is controlled to be-35 ℃ to-40 ℃.

12. The SOF of claim 9₂The preparation method of the gas is characterized in that: in the step 1-1, the solvent is acetonitrile.

13. The SOF of claim 9₂The preparation method of the gas is characterized in that: in the step 1-2, anhydrous KF is added for adsorption reaction, and the adsorption reaction time is 2-30 days.

14. The SOF of claim 13, wherein the SOF comprises a solid-state material₂The preparation method of the gas is characterized in that: the time of the adsorption reaction is 2-20 days.

15. The SOF of claim 13, wherein the SOF comprises a solid-state material₂The preparation method of the gas is characterized in that: the time of the adsorption reaction is 2-10 days.

16. The SOF of claim 9₂The preparation method of the gas is characterized in that: further comprising the steps of 1-3: when KF color does not turn yellow, adsorbed SOF is₂Gas transfer to the SOF₂And storing the mixture in a kettle for later use.

17. SOF₄The preparation system of gas, its characterized in that: the SOF₄The gas preparation system comprises SOF₂Gas inlet duct, fluorine gas duct, SOF₄A reaction kettle and a temperature control device;

the SOF₂Gas inlet duct and said fluorine gas duct and said SOF₄The reaction kettle is connected, the SOF₄The reaction kettle is arranged in the temperature control device;

the SOF₄The gas preparation system further comprises a SOF₄Purification kettle, said SOF₄Reaction kettle and SOF₄The purification kettle is connected with the purification kettle,

the SOF₄The gas preparation system further comprises a SOF₂Gas preparation apparatus, said SOF₂The gas preparation plant comprises a SOF₂Reaction kettle, heating water bath circulating pump, low-temperature circulating pump, constant-pressure dropping funnel, condensing device and SOF₂Purification kettle and SOF₂Storing the kettle;

wherein the SOF₂The reaction kettle is connected with the condensing device, the heating water bath circulating pump and the constant-pressure dropping funnel; the condensing units are respectivelyWith the low-temperature circulating pump and the SOF₂Connecting the purification kettle;

the SOF₂Purification kettle and SOF₂Storage vessel connected, the SOF₂Passing the storage kettle through the SOF₂Air inlet duct and said SOF₄The reaction kettle is connected.

18. The SOF of claim 17, wherein the SOF comprises a solid-state material₄The preparation system of gas, its characterized in that: the SOF₄The gas preparation system further comprises a vacuum evacuation pipeline, wherein the vacuum evacuation pipeline and the SOF are connected₄The reaction kettle is connected, the SOF₄Purification kettle and SOF₄The storage kettle is connected.