CN218909881U - Tetrafluoro oxygen sulfur apparatus for producing - Google Patents

Abstract

The utility model discloses a tetrafluoro-oxy-sulfur production device, which comprises a medium-temperature electrolytic tank, a charcoal reactor, a primary dust remover, a fluorine buffer tank, a secondary dust remover, an SOF4 microchannel reactor, a steel bottle, an S0F2 storage tank, an SOF2 condensation collection tank, an SOF2 synthesis reaction kettle, a two-stage washing circulation tank, a gas-water separator and a flame arrester. The equipment in the utility model divides the tetrafluoro-oxy-sulfur synthesis technology into two steps, namely, firstly synthesizes difluoro-oxy-sulfur through the SOF2 synthesis reaction kettle, and then prepares fluorine gas fluorinated difluoro-oxy-sulfur through the medium-temperature electrolytic tank to synthesize tetrafluoro-oxy-sulfur, so that the raw materials are easy to obtain, the price is low, the oxidation synthesis method using expensive tetrafluoro-sulfur as the raw materials is avoided, the reaction process is mild and controllable, and the high-temperature and high-pressure safety problem of the process for preparing tetrafluoro-oxy-sulfur by oxidizing tetrafluoro-sulfur is avoided.

Description

Tetrafluoro oxygen sulfur apparatus for producing

Technical Field

The utility model relates to the technical field of tetrafluoro oxygen sulfur production, in particular to a tetrafluoro oxygen sulfur production device.

Background

Tetrafluorooxysulfide, molecular formula: SOF4, a colorless, pungent odor gas at room temperature, has previously been found only in sulfur hexafluoride decomposition products, and has been recently reported and artificially synthesized for unknown uses. In recent years, with the continuous development of high-end medicines and functional reagents, particularly after the establishment of revolutionary "click chemistry" theory in the field of chemical synthesis, the performance of tetrafluorooxysulfide has been widely paid attention to and studied. The application of the tetrafluoro-oxysulfide is wide in the application in the medicine industry, and has research reports that the tetrafluoro-oxysulfide has immeasurable application prospects in the aspects of synthesizing innovative medicaments and innovative materials.

However, there is almost no industrial preparation method capable of continuously producing SOF4 in batches at home and abroad, and the literature is only small-scale in the United states, and an SF4 oxidation method is adopted, but the method is a high-temperature high-pressure reaction, has extremely high equipment requirements, has considerable potential safety hazards and is not suitable for large-scale production.

In 2018, there is a patent report that tetrafluorooxysulfide can be synthesized in small amounts in steps of kilogram, which is also a report about a method for preparing tetrafluorooxysulfide for the first time (CN 108128758. B). In the patent, raw materials are produced in steps, then a 10L reaction kettle is used as a reaction container, and the raw materials are put into the reaction kettle for standing reaction, and the reaction is waited for completion. The patent provides a method and a device for producing the gas with a small kilogram level, which have the defects of relatively complex operation, less production quantity, low efficiency, standing and waiting in the reaction process, and incapability of performing any operation to promote the reaction, and the method needs to consume a large amount of electric power and liquid nitrogen, and repeatedly reduces the temperature and heats the operation, so that the energy saving is not facilitated. The production equipment of the method limits the production to be only capable of carrying out kilogram-level small-scale preparation, has low reaction efficiency, has high energy consumption, is not beneficial to the requirement of energy-saving production, and is not suitable for large-scale production.

Disclosure of Invention

Aiming at the technical defects, the utility model aims to provide a tetrafluoro-oxy-sulfur production device, and solves the problems that the existing method for preparing sulfur tetrafluoride is high-temperature and high-pressure reaction, has extremely high equipment requirements and great potential safety hazard, and is not suitable for large-scale production.

In order to solve the technical problems, the utility model adopts the following technical scheme:

the utility model provides tetrafluoro oxygen sulfur production equipment, which comprises a medium-temperature electrolytic tank, a charcoal reactor, a primary dust remover, a fluorine buffer tank, a secondary dust remover, an SOF4 micro-channel reactor, a steel bottle, an S0F2 storage tank, an SOF2 condensation collection tank, an SOF2 synthesis reaction kettle, a two-stage washing circulation tank, a gas-water separator and a flame arrester, wherein the medium-temperature electrolytic tank, the primary dust remover, the fluorine buffer tank, the secondary dust remover and the SOF4 micro-channel reactor are sequentially connected, the SOF2 synthesis reaction kettle, the SOF2 condensation collection tank, the S0F2 storage tank and the SOF4 micro-channel reactor are sequentially connected, the charcoal reactor is connected with the medium-temperature electrolytic tank, and the steel bottle is connected with the SOF2 condensation collection tank.

The utility model has the beneficial effects that: the equipment in the utility model divides the tetrafluoro-oxy-sulfur synthesis technology into two steps, namely, firstly synthesizes difluoro-oxy-sulfur through an SO2 synthesis reaction kettle, and then prepares fluorine gas fluorinated difluoro-oxy-sulfur through a medium-temperature electrolytic tank to synthesize tetrafluoro-oxy-sulfur, SO that the raw materials are easy to obtain, the price is low, the oxidation synthesis method using expensive tetrafluoro-sulfur as the raw materials is avoided, the reaction process is mild and controllable, and the high-temperature and high-pressure safety problem of the process for preparing tetrafluoro-oxy-sulfur by oxidizing tetrafluoro-sulfur is avoided.

Drawings

In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the utility model, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.

FIG. 1 is a schematic structural diagram of a sulfur tetrafluoro oxide production apparatus according to an embodiment of the present utility model;

FIG. 2 is a flow chart of a tetrafluoro oxygen sulfur production apparatus according to an embodiment of the present utility model;

reference numerals illustrate: 1. a medium temperature electrolytic tank; 2. a charcoal reactor; 3. a primary dust remover; 4. a fluorine buffer tank; 5. a secondary dust remover; 6. SOF4 microchannel reactor; 7. a steel cylinder; 8. S0F2 storage tank; 9. SOF2 condensation collection tank; 10. SO2 synthesis reaction kettle; 11. a two-stage water washing circulation tank; 12. a gas-water separator; 13. and a flame arrester.

Detailed Description

The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.

Embodiment 1, as shown in fig. 1 to 2, a tetrafluoro-oxy-sulfur production device comprises a medium-temperature electrolytic tank, a charcoal reactor, a primary dust remover, a fluorine buffer tank, a secondary dust remover, a SOF4 micro-channel reactor, a steel bottle, an S0F2 storage tank, a SOF2 condensation collection tank, a SOF2 synthesis reaction kettle, a two-stage washing circulation tank, a gas-water separator and a flame arrester, wherein the medium-temperature electrolytic tank, the primary dust remover, the fluorine buffer tank, the secondary dust remover and the SOF4 micro-channel reactor are sequentially connected, the SOF2 synthesis reaction kettle, the SOF2 condensation collection tank, the S0F2 storage tank and the SOF4 micro-channel reactor are sequentially connected, the charcoal reactor is connected with the medium-temperature electrolytic tank, and the steel bottle is connected with the SOF2 condensation collection tank, so that the aim of producing tetrafluoro-oxy-sulfur is achieved by recombining the existing device.

Firstly, preparing fluorine gas by utilizing an intermediate-temperature electrolytic tank to electrolyze anhydrous hydrogen fluoride, and then filtering and dedusting by a primary deduster, a fluorine gas buffer tank and a secondary deduster, and then adsorbing and purifying the fluorine gas, and then entering the fluorine gas buffer tank for standby.

And secondly, adding fluorine-containing compounds into a reaction kettle, pouring a proper amount of acetonitrile solvent, heating (0-100 ℃) and stirring to melt, then slowly introducing thionyl chloride into the reaction kettle to react to generate difluoro oxysulfide, and collecting the generated difluoro oxysulfide by a collecting tank and then treating at a low temperature (0-100 ℃) to obtain a pure difluoro oxysulfide product.

Thirdly, putting the difluoro oxysulfide and the fluorine gas into a micro-channel reactor according to a certain proportion at a constant speed, and reacting the difluoro oxysulfide and the fluorine gas at 20-200 ℃ to obtain the final required tetrafluorooxysulfide product.

The reaction equation: sof2+2f2=sof4.

The purity of the tetrafluorooxysulfide produced by the production method of example was examined by thermal conductive gas chromatography (TCD). Specific detection conditions for thermal conductivity gas chromatography (TCD) are as follows:

gas chromatograph: GC-001

Column: H/R2 separation column

Flow rate: 1.0ml/min

Column temperature: 60 DEG C

Mobile phase: SOF4

Detection result: 95% of

The equipment in the utility model divides the tetrafluoro-oxy-sulfur synthesis technology into two steps, namely, firstly synthesizes difluoro-oxy-sulfur through the SOF2 synthesis reaction kettle, and then prepares fluorine gas fluorinated difluoro-oxy-sulfur through the medium-temperature electrolytic tank to synthesize tetrafluoro-oxy-sulfur, so that the raw materials are easy to obtain, the price is low, the oxidation synthesis method using expensive tetrafluoro-sulfur as the raw materials is avoided, the reaction process is mild and controllable, and the high-temperature and high-pressure safety problem of the process for preparing tetrafluoro-oxy-sulfur by oxidizing tetrafluoro-sulfur is avoided.

It will be apparent to those skilled in the art that various modifications and variations can be made to the present utility model without departing from the spirit or scope of the utility model. Thus, it is intended that the present utility model also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (1)

1. The tetrafluoro oxygen sulfur production device is characterized by comprising a medium-temperature electrolytic tank, a charcoal reactor, a primary dust remover, a fluorine buffer tank, a secondary dust remover, a SOF4 micro-channel reactor, a steel bottle, an S0F2 storage tank, a SOF2 condensation collection tank, a SOF2 synthesis reaction kettle, a two-stage washing circulation tank, a gas-water separator and a flame arrester, wherein the medium-temperature electrolytic tank, the primary dust remover, the fluorine buffer tank, the secondary dust remover and the SOF4 micro-channel reactor are sequentially connected, the SOF2 synthesis reaction kettle, the SOF2 condensation collection tank, the S0F2 storage tank and the SOF4 micro-channel reactor are sequentially connected, the charcoal reactor is connected with the medium-temperature electrolytic tank, and the steel bottle is connected with the SOF2 condensation collection tank.

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