CN217962562U - Reactor for efficiently preparing sulfur tetrafluoride - Google Patents
Reactor for efficiently preparing sulfur tetrafluoride Download PDFInfo
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- CN217962562U CN217962562U CN202222412657.1U CN202222412657U CN217962562U CN 217962562 U CN217962562 U CN 217962562U CN 202222412657 U CN202222412657 U CN 202222412657U CN 217962562 U CN217962562 U CN 217962562U
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Abstract
The utility model relates to a reactor of high-efficient preparation sulfur tetrafluoride, including reactor main part and the reinforced mechanism of sulphur, the entrance point of reactor main part is provided with the iodine pentafluoride feed inlet, the exit end of reactor main part is provided with gas outlet, a plurality of baffles have been installed to the equidistance on the interior roof of reactor main part, the height of baffle equals 1/2 of reactor main part height. The utility model discloses the effect of well baffle has been equivalent to having established ties many horizontal reactors, filler in the reactor floats on sulphur liquid upper portion, the liquid sulphur of surface adhesion, gas-liquid double-phase area of contact has been increased, the reaction efficiency is improved, sulfur level gauge on the reactor can observe the sulphur liquid level in the reactor directly perceivedly simultaneously, with quantitative jar heating and the accurate reinforced solid sulphur of screw feed pump chain control, but degree of automation is high, and the operation is simple, the reinforced problem of blockking up the pipeline of sulphur has also been solved in the setting of quantitative jar and quantitative jar heating tile, the continuity of reaction has been improved.
Description
Technical Field
The utility model belongs to the technical field of sulfur tetrafluoride preparation, especially, a reactor of high-efficient preparation sulfur tetrafluoride.
Background
Sulfur tetrafluoride is the most widely used selective organic fluorinating agent at present, which can selectively fluorinate hydroxyl and carbonyl, and has an irreplaceable position in the production of fine chemicals, liquid crystal materials and high-end pharmaceutical industries. In addition, the sulfur tetrafluoride can also be used as an electron gas, chemical vapor deposition, plasma etching and the like.
At present, four methods for preparing sulfur tetrafluoride are available, namely a hydrogen fluoride fluorination method, an organic base hydrofluoride fluorination method, a fluorine gas fluorination method and a non-metal fluoride fluorination method. The fluorine gas fluorination method is adopted to prepare sulfur tetrafluoride products in foreign reports, the nonmetal fluoride fluorination method is mainly adopted to prepare sulfur tetrafluoride in China at present, and most of nonmetal fluorides adopted are iodine pentafluoride.
In the publication of: CN211310840U discloses a sulfur tetrafluoride synthesis reactor, which realizes accurate control of the reactor body temperature through hot liquid circulation in a jacket, and the subsequent treatment is simple, but the reactor still has the problems of low reaction efficiency, incomplete reaction, waste of raw materials, and incapability of accurately measuring the sulfur liquid level in the reactor.
SUMMERY OF THE UTILITY MODEL
The utility model provides a its technical problem take following technical scheme to realize:
the utility model provides a reactor of high-efficient preparation sulfur tetrafluoride, includes reactor main part and the reinforced mechanism of sulphur, the entrance point of reactor main part is provided with the iodine pentafluoride feed inlet, the exit end of reactor main part is provided with gas outlet, a plurality of baffles have been installed to the equidistance on the interior roof of reactor main part, the height of baffle equals the 1/2 of reactor main part height.
The sulfur charging mechanism comprises a sulfur storage tank, a spiral charging pump and a quantitative tank, wherein a liquid sulfur charging port is arranged at the inlet end of the reactor main body, the quantitative tank is connected between the spiral charging pump and the liquid sulfur charging port, and the sulfur storage tank is connected with the spiral charging pump.
Heating tiles are arranged on the quantitative tank and the liquid sulfur feeding port.
The volume of the quantitative tank is equal to the length of the reactor body multiplied by the diameter of the reactor body multiplied by 1-10mm.
The reactor main body is provided with a heating tile.
And pressure transmitters are arranged at the inlet end and the outlet end of the reactor main body.
And a temperature transmitter is arranged on the reactor main body.
And a sulfur liquid level meter is arranged on the reactor main body.
A plurality of fillers are arranged in the reactor main body.
The filler is one or two of stainless steel, monel and nickel pall rings and theta rings.
The utility model has the advantages that:
1. the baffle in the reactor is equivalent to a plurality of horizontal reactors connected in series, the equipment volume and other accessory investment are reduced, the cost is reduced, the filler in the reactor floats on the upper part of the sulfur liquid, the liquid sulfur is attached to the surface, the contact area of gas-liquid two phases is increased, and the reaction efficiency is improved.
2. The pressure sensor that reactor both ends were equipped with and the level gauge of one side setting can directly perceivedly observe sulphur liquid level in the reactor, with quantitative jar heating and the accurate reinforced solid sulphur of screw feed pump chain control, but degree of automation is high, easy operation, quantitative jar and quantitative jar heating tile set up the problem of the reinforced jam pipeline of sulphur also to have solved, have improved the continuity of reaction.
Drawings
Fig. 1 is a schematic view of the overall structure.
Wherein: 1. a reactor main body; 2. an iodine pentafluoride feed inlet; 3. a gas outlet; 4. a baffle plate; 5. a sulphur storage tank; 6. a screw feed pump; 7. a dosing tank; 8. a liquid sulfur feed port; 9. heating the tile; 10. a pressure transmitter; 11. a temperature transmitter; 12. a sulphur level gauge; 13. and (4) filling.
Detailed Description
The utility model is described in detail with the accompanying drawings as follows:
as shown in figure 1, the utility model provides a high-efficient preparation sulfur tetrafluoride's reactor, including the reinforced mechanism of reactor main part 1 and sulphur, the reinforced mechanism of sulphur is used for adding liquid sulphur to reactor main part 1, and the entrance point of reactor main part 1 is provided with iodine pentafluoride feed inlet 2, and the exit end of reactor main part 1 is provided with gas outlet 3, and a plurality of baffles 4 have been installed to the equidistance on the interior roof of reactor main part 1, and the height of baffle 4 equals 1/2 of reactor main part 1 height, installs sulphur level gauge 12 on the reactor main part 1.
When the reaction is carried out, liquid sulfur is added into the reactor main body 1 through the sulfur feeding mechanism, in the process, the liquid level of the sulfur can be monitored through the sulfur liquid level meter 12, when the sulfur liquid level meter 12 shows that the liquid sulfur reaches 1/2 of the height of the reactor main body 1, the sulfur feeding mechanism stops feeding, at the moment, the liquid level of the liquid sulfur is in contact with the baffle plates 4, relatively closed reaction spaces are formed between the adjacent baffle plates 4, a plurality of horizontal reactors are connected in series, iodine pentafluoride is added from the iodine pentafluoride feeding hole 2, after the liquid sulfur enters the reactor main body 1, the gasification of the iodine pentafluoride is reacted with the sulfur, along with the continuous reaction, the pressure rises, the liquid sulfur in the reaction spaces can be gradually compressed to move towards the outlet end of the reactor main body 1, when the liquid level of the sulfur is lower than the baffle plates 4, the reacted gas can enter the next reaction space to be reacted in sequence, in the continuous and stable operation process of the reaction, the inlet end of the reactor main body 1 is pressed to the outlet end pressure, the full reaction can be continuously promoted, and the utilization rate of the iodine pentafluoride is improved.
Specifically, the utility model discloses in, the reinforced mechanism of sulphur includes sulphur storage tank 5, screw feed pump 6 and quantitative jar 7, and the entrance point of reactor main part 1 is provided with liquid sulphur charge door 8, and quantitative jar 7 connects to be located between screw feed pump 6 and the liquid sulphur charge door 8, and sulphur storage tank 5 meets with screw feed pump 6, and the volume of quantitative jar 7 equals that 1 length of reactor main part multiplies 1 diameter of reactor main part and multiplies 1-10mm, and quantitative jar 7 and liquid sulphur charge door 8 facial make-up are equipped with heating tile 9.
Add in the sulphur storage tank 5 solid sulphur, screw feed pump 6 can carry solid sulphur to quantitative jar 7 in, install heating tile 9 on the quantitative jar 7, can heat the solid sulphur in the quantitative jar 7 and make it trun into liquid, then liquid sulphur gets into to reactor main part 1 through liquid sulphur charge door 8, also install heating tile 9 on the liquid sulphur charge door, can make liquid sulphur charge door 8 be in suitable temperature, the solidification leads to the situation of jam when avoiding liquid sulphur from the well process.
Specifically, the utility model discloses in, all install pressure transmitter 10 on the entrance point of reactor main part 1 and the exit end, pressure indicator is equipped with between the pressure transmitter 10, be used for detecting and feeding back the pressure information in the pressure reactor main part 1 and give outside controller, again by heating tile 9 on controller control ration jar 7 and the liquid sulphur charge door 8, and simultaneously, heating tile 9 and screw feed pump 6 on sulphur level gauge 12 and the ration jar 7 are chain, sulphur level information in sulphur level gauge 12 feedback reactor main part 1, when the sulphur liquid level is less than 1/2, by the heating tile 9 heating on the controller control ration jar 7, start screw feed pump 6 simultaneously and add solid sulphur in to the ration jar 7.
Specifically, in the utility model, a plurality of fillers 13 are arranged in the reactor main body 1, the fillers 3 are stainless steel, monel, nickel pall rings or theta rings, preferably, the fillers 13 are monel pall rings. After the liquid sulfur is added into the reactor main body 1, the filler 13 floats on the surface, and the liquid sulfur is attached to the surface, so that the contact area of gas-liquid two phases is increased, and further, the reaction efficiency is improved.
Specifically, the utility model discloses in, install temperature transmitter 11 on the reactor main part 1 for the reaction temperature in the monitoring reactor main part 1, the guarantee is stable, safe reacts.
In summary, the overall working flow of the reactor is as follows:
(1) Adding a filler 13 into the reactor main body 1, starting a heating tile 9 on the reactor main body 1 for preheating, and controlling the temperature of the reactor main body 1 to reach a reaction temperature;
(2) Adding solid sulfur into a sulfur storage tank 5, starting a quantitative tank 7 and a heating tile 9 on a liquid sulfur feed port 8, feeding sulfur into a spiral feed pump 6 by feedback control of a sulfur liquid level meter 12 because the sulfur liquid level does not exist in a reactor main body 1, controlling the spiral feed pump 6 to stop feeding when the sulfur liquid level meter 12 displays that the sulfur liquid level reaches 1/2, and stopping the heating tile 9 on the quantitative tank 7;
(3) Opening the iodine pentafluoride feed inlet 2, allowing iodine pentafluoride to enter the reactor main body 1 for gasification to react with the liquid sulfur on the upper liquid level of each section of liquid sulfur and the surface of the filler 13, increasing the reaction pressure, gradually compressing the liquid sulfur to move towards an outlet, and allowing the reacted gas to enter the next stage for reaction in sequence when the liquid level is lower than the baffle 4;
(4) Along with the reaction, liquid sulfur is consumed, when there is not pressure difference in reactor main part 1 both ends pressure, it indicates that liquid sulfur liquid level is less than baffle 4, the reactor effect of establishing ties became invalid, 12 demonstration liquid levels of sulphur level gauge were less than 1/2 this moment, pressure transmitter 11 and 12 feedback control quantitative jar 7 of sulphur level gauge, the heating tile 9 on the liquid sulphur charge door 8 heats and 6 start-up feed supplement sulphur of screw feed pump, reach balanced back iodine pentafluoride and the equal continuous stable feeding of sulphur, stable continuous high-efficient preparation sulfur tetrafluoride.
(5) And finally, discharging the reacted gas from a gas outlet 3, and condensing, purifying and collecting the gas to obtain the sulfur tetrafluoride.
By utilizing the reactor recorded by the utility model, 99.94 percent of sulfur tetrafluoride product can be prepared, and the interest rate of iodine pentafluoride is converted to more than 99 percent.
It should be emphasized that the embodiments described herein are illustrative and not restrictive, and thus the present invention includes but is not limited to the embodiments described in the detailed description, as well as other embodiments derived from the technical solutions of the present invention by those skilled in the art, which also belong to the scope of the present invention.
Claims (10)
1. The utility model provides a reactor of high-efficient preparation sulfur tetrafluoride, includes reactor main part and the reinforced mechanism of sulphur, the entrance point of reactor main part is provided with the iodine pentafluoride feed inlet, the exit end of reactor main part is provided with gas outlet, its characterized in that: a plurality of baffles are equidistantly arranged on the inner top wall of the reactor main body, and the height of each baffle is equal to 1/2 of the height of the reactor main body.
2. The reactor for efficiently preparing sulfur tetrafluoride according to claim 1, wherein: the sulfur feeding mechanism comprises a sulfur storage tank, a spiral feeding pump and a quantitative tank, a liquid sulfur feeding port is arranged at the inlet end of the reactor main body, the quantitative tank is connected between the spiral feeding pump and the liquid sulfur feeding port, and the sulfur storage tank is connected with the spiral feeding pump.
3. The reactor for efficiently preparing sulfur tetrafluoride according to claim 2, wherein: heating tiles are arranged on the quantitative tank and the liquid sulfur feeding port.
4. The reactor for efficiently producing sulfur tetrafluoride according to claim 2, wherein: the volume of the quantitative tank is equal to the length of the reactor body multiplied by the diameter of the reactor body multiplied by 1-10mm.
5. The reactor for efficiently preparing sulfur tetrafluoride according to claim 1, wherein: the reactor main body is provided with a heating tile.
6. The reactor for efficiently producing sulfur tetrafluoride according to claim 1, wherein: and pressure transmitters are arranged at the inlet end and the outlet end of the reactor main body.
7. The reactor for efficiently preparing sulfur tetrafluoride according to claim 1, wherein: and a temperature transmitter is arranged on the reactor main body.
8. The reactor for efficiently preparing sulfur tetrafluoride according to claim 1, wherein: and a sulfur liquid level meter is arranged on the reactor main body.
9. The reactor for efficiently preparing sulfur tetrafluoride according to claim 1, wherein: the reactor main body is provided with a plurality of fillers.
10. The reactor for efficiently producing sulfur tetrafluoride according to claim 9, wherein: the filler is one or two of pall rings and theta rings made of stainless steel, monel and nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222412657.1U CN217962562U (en) | 2022-09-13 | 2022-09-13 | Reactor for efficiently preparing sulfur tetrafluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222412657.1U CN217962562U (en) | 2022-09-13 | 2022-09-13 | Reactor for efficiently preparing sulfur tetrafluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN217962562U true CN217962562U (en) | 2022-12-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222412657.1U Active CN217962562U (en) | 2022-09-13 | 2022-09-13 | Reactor for efficiently preparing sulfur tetrafluoride |
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| Country | Link |
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| CN (1) | CN217962562U (en) |
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- 2022-09-13 CN CN202222412657.1U patent/CN217962562U/en active Active
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