A preparation process and preparation device for high-purity hydrogen sulfide

Abstract

The present invention provides a process and apparatus for preparing high-purity hydrogen sulfide, relating to the technical field of hydrogen sulfide preparation. The process comprises obtaining high-purity sulfur, melting the high-purity sulfur in a sulfur melting kettle to produce liquid high-purity sulfur, preparing hydrogen gas and heating the hydrogen gas, and then sending the liquid high-purity sulfur and the heated hydrogen gas to a reaction tower for reaction to produce high-purity hydrogen sulfide gas. In the present invention, the use of high-purity sulfur and high-purity hydrogen to prepare hydrogen sulfide can reduce the generation of impurity gases and improve the purity of the hydrogen sulfide gas.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrogen sulfide preparation, and in particular to a preparation process and a preparation device for high-purity hydrogen sulfide. Background Art

[0002] Thiol compounds are a class of organic compounds containing a thiol (-SH) functional group. They are widely used in a variety of fields. During their preparation, hydrogen sulfide can be used as a sulfur source to introduce thiols. To ensure high yields, large quantities of high-purity hydrogen sulfide are required.

[0003] The Chinese patent with the authorization announcement number CN115535967B discloses a method for preparing hydrogen sulfide, which comprises reacting a natural mineral containing pyrrhotite with sulfuric acid to generate hydrogen sulfide gas. The present invention selects pyrrhotite with high reactivity to react with sulfuric acid. Sodium ions will not be introduced into the reaction system, and the subsequent treatment is relatively easy. Moreover, the natural mineral containing pyrrhotite is cheap and widely available. It is often associated with heavy non-ferrous metals such as copper, lead, and zinc. Therefore, it is easy to obtain it in the copper, lead, and zinc beneficiation process, thereby realizing the comprehensive utilization of resources and reducing the overall production cost. The hydrogen sulfide finally prepared can be used for the removal of heavy metal precipitation in wastewater or sewage systems during non-ferrous metal smelting. The method provided by the present invention is particularly suitable for use in non-ferrous metallurgical enterprises. In addition, the present invention makes full use of the magnetism of pyrrhotite and sets an alternating magnetic field outside the tubular reactor to achieve unpowered stirring.

[0004] However, in the above-mentioned hydrogen sulfide preparation method, since natural minerals are reacted with sulfuric acid, the hydrogen sulfide gas generated during the reaction will be mixed with impurity gases such as carbon dioxide and sulfur dioxide, and will also produce products such as iron-containing sulfates, thereby reducing the purity of the hydrogen sulfide. Summary of the Invention

[0005] The present invention provides a preparation process and a preparation device for high-purity hydrogen sulfide, which are used to solve the technical problem in the current hydrogen sulfide preparation method that the generated hydrogen sulfide gas is mixed with impurity gases, thereby reducing the purity of the hydrogen sulfide.

[0006] In order to solve the above technical problems, the present invention discloses a process for preparing high-purity hydrogen sulfide, comprising:

[0007] Obtain high-purity sulfur, add the high-purity sulfur into a sulfur melting kettle and melt it to obtain liquid high-purity sulfur;

[0008] preparing hydrogen and heating the hydrogen;

[0009] Liquid high-purity sulfur and heated hydrogen are sent to a reaction tower to react and produce high-purity hydrogen sulfide gas.

[0010] Preferably, the high-purity sulfur is in granular or powder form.

[0011] Preferably, the purity of hydrogen is greater than or equal to 99.9%.

[0012] The present invention also discloses a device for preparing high-purity hydrogen sulfide, which adopts the above-mentioned high-purity hydrogen sulfide preparation process to prepare high-purity hydrogen sulfide. The device includes a sulfur melting kettle, a reaction tower and a heater. The output end of the sulfur melting kettle is connected to the reaction tower through a liquid inlet pipe, and a first liquid sulfur pump is provided on the liquid inlet pipe. The output end of the heater is connected to the reaction tower through an air inlet pipe, and an air inlet pump is provided on the air inlet pipe.

[0013] Preferably, a stirring mechanism is provided in the molten sulfur kettle.

[0014] Preferably, a liquid return pipe is provided at the bottom of the reaction tower, one end of the liquid return pipe away from the reaction tower is connected to the sulfur melting kettle, and a second liquid sulfur pump is provided on the liquid return pipe.

[0015] Preferably, it also includes a hydrogen sulfide collection component, which includes a condensation tank and a hydrogen sulfide collection cylinder. Three condensation tanks are provided, and a condensation mechanism is provided in the condensation tank. Two adjacent condensation tanks are connected by a connecting pipe. The inlet of the condensation tank close to the reaction tower is connected to the top of the reaction tower through a first collecting pipe. A first collecting pump is provided on the first collecting pipe. A drain pipe is provided at the bottom of the condensation tank. The lower end of the drain pipe is connected to the second collecting pipe. The output end of the second collecting pipe is connected to the hydrogen sulfide collection cylinder. A second collecting pump is provided near the output end of the second collecting pipe.

[0016] Preferably, the outlet of the condensation tank away from the reaction tower is connected to the input end of the heater through a hydrogen recovery pipe, and a hydrogen recovery pump is provided on the hydrogen recovery pipe.

[0017] Preferably, a diverter ring is provided in the reaction tower, and the diverter ring has an annular structure. The outer wall of the diverter ring is connected to the inner wall of the reaction tower, an annular cavity is provided in the diverter ring, a plurality of liquid spray holes are provided at the bottom of the diverter ring, and the upper end of the liquid spray hole is connected to the annular cavity, an annular cylinder is provided above the diverter ring, and the outer wall of the annular cylinder is connected to the inner wall of the reaction tower through a connecting plate, a separating ring is provided in the annular cylinder, and the central axis of the separating ring is on the same straight line as the central axis of the annular cylinder. The separating ring divides the annular cylinder into a liquid inlet chamber and a mixing chamber, and the mixing chamber is located on the inner side of the separating ring, and a plurality of connecting holes are provided at the lower position of the separating ring, and a one-way valve is provided in the connecting hole, and the liquid inlet chamber is connected to the mixing chamber through the connecting hole, and a delivery hole is provided at the bottom of the mixing chamber, and a delivery pipe is provided at the lower end of the delivery hole, and the delivery pipe is connected to the annular cavity away from one end of the annular cylinder, and a liquid supply pipe is provided at the upper end of the annular cylinder, one end of the liquid supply pipe is connected to the liquid inlet chamber, and the other end of the liquid supply pipe is connected to the liquid inlet pipe.

[0018] Preferably, the upper end of the liquid spray hole is funnel-shaped.

[0019] The technical solution of the present invention has the following advantages: The present invention provides a process and apparatus for preparing high-purity hydrogen sulfide, relating to the technical field of hydrogen sulfide preparation. The process comprises obtaining high-purity sulfur, melting the high-purity sulfur in a sulfur melting kettle to produce liquid high-purity sulfur, preparing hydrogen gas and heating the hydrogen gas, and then sending the liquid high-purity sulfur and the heated hydrogen gas to a reaction tower for reaction to produce high-purity hydrogen sulfide gas. In the present invention, the use of high-purity sulfur and high-purity hydrogen gas to prepare hydrogen sulfide can reduce the generation of impurity gases and improve the purity of the hydrogen sulfide gas.

[0020] Other features and advantages of the present invention will be described in the following description, and in part will become apparent from the description, or will be understood by practicing the present invention. The purpose and other advantages of the present invention can be realized and obtained by the devices particularly pointed out in the written description and the accompanying drawings.

[0021] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0023] Figure 1 This is a process flow chart for preparing high-purity hydrogen sulfide according to the present invention;

[0024] Figure 2 This is a schematic diagram of the overall structure of a high-purity hydrogen sulfide preparation device of the present invention;

[0025] Figure 3 Schematic diagram of the internal structure of the reaction tower in the present invention;

[0026] Figure 4 For the present invention Figure 3 A magnified view of the structure at center A;

[0027] Figure 5 This is a schematic diagram of the push rod in the present invention pushing the sealing baffle downward;

[0028] Figure 6 For the present invention Figure 5 A magnified view of the structure at point B in the middle;

[0029] Figure 7 It is a bottom view of the diverter ring in the present invention.

[0030] In the figure: 1. molten sulfur kettle; 2. reaction tower; 3. heater; 4. condenser; 5. hydrogen sulfide collecting cylinder; 6. diverter ring; 7. annular cavity; 8. spray hole; 9. annular cylinder; 10. connecting plate; 11. separating ring; 12. liquid inlet chamber; 13. mixing chamber; 14. delivery pipe; 15. liquid supply pipe; 16. diverter plate; 17. nozzle; 18. sealing baffle; 19. mounting hole; 20. connecting column; 21. connecting spring; 22. electric push rod; 23. push rod; 24. first annular push plate; 25. second annular push plate; 26. reset spring; 27. annular push block; 28. moving disk; 29. ​​first push rod; 30. second push rod; 31. sliding groove; 32. sliding plate; 33. block; 34. compression spring. DETAILED DESCRIPTION

[0031] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0032] In addition, in the present invention, descriptions such as "first" and "second" are only used for descriptive purposes, and do not specifically refer to the order or sequence, nor are they used to limit the present invention. They are only used to distinguish components or operations described with the same technical terms, and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions and technical features between the various embodiments can be combined with each other, but this must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0033] Example 1

[0034] The present invention provides a process for preparing high-purity hydrogen sulfide. Figure 1 Shown, including:

[0035] Obtain high-purity sulfur, add the high-purity sulfur into the sulfur melting kettle 1 and melt it to obtain liquid high-purity sulfur;

[0036] preparing hydrogen and heating the hydrogen;

[0037] The liquid high-purity sulfur and the heated hydrogen are sent to the reaction tower 2 to react and produce high-purity hydrogen sulfide gas;

[0038] High-purity sulfur comes in granular or powder form;

[0039] The purity of hydrogen is greater than or equal to 99.9%.

[0040] The working principle and beneficial effects of the above technical solution are as follows: during preparation, high-purity sulfur is first prepared, the purity of the high-purity sulfur is at least 99.9%, and then the high-purity sulfur is added to the sulfur melting kettle 1 for melting to obtain liquid high-purity sulfur; then hydrogen is prepared, the purity of the hydrogen is not less than 99.9%, and the hydrogen is heated to prevent the hydrogen temperature entering the reaction tower 2 from being too low and affecting the reaction process, and then the liquid high-purity sulfur and the heated hydrogen are sent to the reaction tower 2 for reaction to obtain high-purity hydrogen sulfide gas. In the above solution, high-purity sulfur and high-purity hydrogen are used to prepare hydrogen sulfide, and the obtained hydrogen sulfide gas is not easily mixed with impurity gases such as carbon dioxide and sulfur dioxide, which reduces the generation of impurity gases and does not produce by-products such as iron-containing sulfates. Finally, high-purity hydrogen sulfide gas is obtained, the purity of the hydrogen sulfide gas is improved, and it is conducive to large-scale use in industrial production.

[0041] Example 2

[0042] On the basis of the above embodiment 1, Figure 2-Figure 7 As shown, an embodiment of the present invention also provides a device for preparing high-purity hydrogen sulfide, including: a molten sulfur kettle 1, a reaction tower 2 and a heater 3, the output end of the molten sulfur kettle 1 is connected to the reaction tower 2 through a liquid inlet pipe, and a first liquid sulfur pump is provided on the liquid inlet pipe, and the output end of the heater 3 is connected to the reaction tower 2 through an air inlet pipe, and an air inlet pump is provided on the air inlet pipe.

[0043] The working principle and beneficial effects of the above technical solution are as follows: high-purity hydrogen sulfide is prepared by using a preparation device, firstly, the prepared high-purity sulfur is added into the sulfur melting kettle 1, the temperature in the sulfur melting kettle 1 is maintained at 300-500°C to ensure that the high-purity sulfur is fully melted, and at the same time, the prepared high-purity hydrogen is passed into the heater 3 for preheating, the preheating temperature can be set by the user, and then the liquid high-purity sulfur is transported to the reaction tower 2 through the liquid inlet pipe by the first liquid sulfur pump, and the preheated hydrogen is passed into the reaction tower 2 by the air inlet pump, and the reaction tower 2 is heated. At a temperature of not less than 300° C., liquid high-purity sulfur and hydrogen react in the high-temperature environment of reaction tower 2 to produce hydrogen sulfide gas. During the preparation process, high-purity sulfur and high-purity hydrogen are used to prepare hydrogen sulfide. The produced hydrogen sulfide gas is not easily mixed with impurity gases such as carbon dioxide and sulfur dioxide, thereby reducing the generation of impurity gases and preventing the generation of by-products such as iron-containing sulfates. Ultimately, high-purity hydrogen sulfide gas is obtained. By preheating the hydrogen, the temperature difference between the hydrogen and the liquid high-purity sulfur can be reduced, thereby making the reaction more complete.

[0044] Example 3

[0045] On the basis of Example 2, a stirring mechanism is provided in the molten sulfur kettle 1 .

[0046] The working principle and beneficial effects of the above technical solution are: the high-purity sulfur in the sulfur melting kettle 1 can be stirred by the stirring mechanism, so that the high-purity sulfur is fully melted, thereby improving the melting effect and melting efficiency.

[0047] Example 4

[0048] On the basis of Example 2 or 3, a liquid return pipe is provided at the bottom of the reaction tower 2, the end of the liquid return pipe away from the reaction tower 2 is connected to the sulfur melting kettle 1, and a second liquid sulfur pump is provided on the liquid return pipe.

[0049] The working principle and beneficial effects of the above technical solution are as follows: unreacted liquid high-purity sulfur flows to the bottom of the reaction tower 2, and a liquid level monitoring device is provided on the reaction tower 2. The liquid level monitoring device is used to monitor the liquid level of the liquid high-purity sulfur in the reaction tower 2. A controller is provided outside the reaction tower 2, and the controller is electrically connected to the liquid level monitoring device and the second liquid sulfur pump respectively. When the liquid level of the liquid high-purity sulfur in the reaction tower 2 is higher than the preset liquid level, the controller outside the reaction tower 2 controls the second liquid sulfur pump to start. The second liquid sulfur pump can extract the liquid high-purity sulfur in the reaction tower 2 to the return pipe and transport it to the sulfur melting kettle 1 through the return pipe, which is conducive to the reuse of the liquid high-purity sulfur. When the liquid level of the liquid high-purity sulfur in the reaction tower 2 reaches the lowest liquid level, the second liquid sulfur pump automatically stops to avoid extracting all the liquid high-purity sulfur and prevent the gas in the reaction tower 2 from entering the sulfur melting kettle 1.

[0050] Example 5

[0051] On the basis of any one of Examples 2-4, Figure 2 As shown, it also includes a hydrogen sulfide collection component, which includes a condensation tank 4 and a hydrogen sulfide collection cylinder 5. Three condensation tanks 4 are provided, and a condensation mechanism is provided in the condensation tank 4. Two adjacent condensation tanks 4 are connected by a connecting pipe. The inlet of the condensation tank 4 close to the reaction tower 2 is connected to the top of the reaction tower 2 through a first collecting pipe. A first collecting pump is provided on the first collecting pipe. A discharge pipe is provided at the bottom of the condensation tank 4. The lower end of the discharge pipe is connected to the second collecting pipe. The output end of the second collecting pipe is connected to the hydrogen sulfide collection cylinder 5. A second collecting pump is provided near the output end of the second collecting pipe.

[0052] The outlet of the condensation tank 4 away from the reaction tower 2 is connected to the input end of the heater 3 through a hydrogen recovery pipe, and a hydrogen recovery pump is provided on the hydrogen recovery pipe.

[0053] The working principle and beneficial effects of the above technical solution are as follows: high-purity hydrogen sulfide gas is generated in the reaction tower 2, but a small amount of unreacted hydrogen is still mixed in the high-purity hydrogen sulfide gas. Therefore, a hydrogen sulfide collecting component is provided to collect the prepared high-purity hydrogen sulfide. Specifically, the first collecting pump is started, and the first collecting pump can extract the gas in the reaction tower 2 into the first condenser 4 through the first collecting pipe. The gas passes through the first condenser 4, the second condenser 4, and the third condenser 4 in sequence. The high-purity hydrogen sulfide gas in the gas is liquefied into hydrogen sulfide liquid and flows to the second collecting pipe through the drain pipe. The second collecting pump is turned on to extract the hydrogen sulfide liquid in the second collecting pipe into the hydrogen sulfide collecting cylinder 5 for collection, and finally the high-purity hydrogen sulfide liquid is collected. The mixed hydrogen enters the hydrogen recovery pipe through the outlet of the condenser 4 after passing through the third condenser 4, and flows to the heater 3 for heating under the action of the hydrogen recovery pump. This not only realizes the separation of hydrogen and hydrogen sulfide, further improves the purity of the hydrogen sulfide liquid, but also realizes the recycling of hydrogen, achieves the effect of energy saving, and reduces In order to reduce the preparation cost, a hydrogen inlet is also provided on the heater 3, through which hydrogen can be introduced to ensure the amount of hydrogen required for production. A condensing mechanism is provided in the condensing tank 4, which includes a spiral cooling tube. A coolant flows in the spiral cooling tube. The coolant is continuously refrigerated and circulated to refrigerate the hydrogen sulfide gas passing through, thereby reducing the temperature of the hydrogen sulfide gas and gradually condensing the hydrogen sulfide gas into hydrogen sulfide liquid. From left to right, the temperature in the first condensing tank 4 is maintained at -10°C to 0°C, and the temperature in the second condensing tank 4 is maintained at - The temperature in the third condenser 4 is maintained at -45°C to -35°C, and the temperature in the third condenser 4 is maintained at -85°C to -75°C. The hydrogen sulfide gas flowing therethrough is gradually cooled so that the hydrogen sulfide gas is fully liquefied and finally collected in the hydrogen sulfide collecting cylinder 5, while the mixed hydrogen flows into the hydrogen recovery pipe in gaseous form through the outlet of the third condenser 4, thereby achieving the separation of hydrogen sulfide and hydrogen, ensuring the purity of the hydrogen sulfide liquid in the hydrogen sulfide collecting cylinder 5, and retaining the hydrogen sulfide liquid in the second collecting pipe, which can prevent hydrogen from mixing into the hydrogen sulfide collecting cylinder 5.

[0054] Example 6

[0055] On the basis of any one of Examples 2-5, Figure 3-Figure 7As shown, a diverter ring 6 is provided in the reaction tower 2, and the diverter ring 6 is annular in structure. The outer wall of the diverter ring 6 is connected to the inner wall of the reaction tower 2. An annular cavity 7 is provided in the diverter ring 6. A plurality of liquid spray holes 8 are provided at the bottom of the diverter ring 6. The upper end of the liquid spray hole 8 is connected to the annular cavity 7. An annular cylinder 9 is provided above the diverter ring 6. The outer wall of the annular cylinder 9 is connected to the inner wall of the reaction tower 2 through a connecting plate 10. A separator ring 11 is provided in the annular cylinder 9. The central axis of the separator ring 11 is in the same straight line as the central axis of the annular cylinder 9. The separator ring 11 divides the inner wall of the annular cylinder 9 into two parts. The partition is a liquid inlet chamber 12 and a mixing chamber 13. The mixing chamber 13 is located inside the separating ring 11. A plurality of communicating holes are provided at the lower position of the separating ring 11. A one-way valve is provided in the communicating hole. The liquid inlet chamber 12 is connected to the mixing chamber 13 through the communicating hole. A delivery hole is provided at the bottom of the mixing chamber 13. A delivery pipe 14 is provided at the lower end of the delivery hole. The delivery pipe 14 is connected to the annular cavity 7 at one end away from the annular cylinder 9. A liquid supply pipe 15 is provided at the upper end of the annular cylinder 9. One end of the liquid supply pipe 15 is connected to the liquid inlet chamber 12, and the other end of the liquid supply pipe 15 is connected to the liquid inlet pipe.

[0056] The upper end of the liquid spray hole 8 is funnel-shaped.

[0057] The working principle and beneficial effects of the above technical solution are as follows: during preparation, liquid high-purity sulfur first flows into the liquid supply pipe 15 through the liquid inlet pipe. The liquid supply pipe 15 adopts a telescopic pipe. The liquid high-purity sulfur flows into the liquid inlet chamber 12 through the liquid supply pipe 15, then enters the mixing chamber 13 through the connecting hole, and is then transported to the annular cavity 7 of the diverter ring 6 through the delivery pipe 14, and finally sprayed downward through the spray hole 8. The liquid high-purity sulfur can be dispersed and flowed out through the diverter ring 6, thereby increasing the contact area between the liquid high-purity sulfur and the hydrogen, facilitating the full reaction of the liquid high-purity sulfur with the hydrogen in the reaction tower 2, and improving the reaction rate. In addition, the liquid high-purity sulfur droplets can quickly diffuse in the hydrogen, so that the high-purity sulfur and hydrogen are mixed more evenly. A plurality of spray holes 8 are provided, and the plurality of spray holes 8 are distributed in a ring array at the bottom of the diverter ring 6. The liquid high-purity sulfur can be uniformly discharged through the plurality of spray holes 8. The upper end of the spray hole 8 is configured in a funnel shape to prevent the liquid high-purity sulfur from remaining in the liquid inlet chamber 12.

[0058] Example 7

[0059] On the basis of Example 6, Figure 3As shown, a diverter disk 16 is provided below the diverter ring 6, an air cavity is provided in the diverter disk 16, the air inlet pipe is connected to the air cavity through the air supply pipe, a plurality of nozzles 17 are provided on the periphery of the diverter disk 16, one end of the nozzle 17 is connected to the air cavity, a sealing baffle 18 is provided on the top of the diverter disk 16, and the sealing baffle 18 is connected to the diverter ring 6 through a connecting mechanism, and the connecting mechanism includes a plurality of mounting holes 19 provided inside the diverter disk 16, a connecting column 20 is slidingly provided in the mounting hole 19, the connecting column 20 is connected to the top wall of the mounting hole 19 through a connecting spring 21, and the lower end of the connecting column 20 is connected to the upper surface of the sealing baffle 18, an electric push rod 22 is provided on the top of the reaction tower 2, a push rod 23 is provided at the output end of the electric push rod 22, and the lower end of the push rod 23 extends to the center of the annular cylinder 9.

[0060] The working principle and beneficial effects of the above technical solution are as follows: in order to further increase the reaction rate, a diverter disk 16 is provided below the diverter ring 6, and hydrogen enters the gas cavity through a retractable gas supply pipe, and then is ejected through a plurality of nozzles 17. The direction of hydrogen ejection from the nozzle 17 intersects with the flow direction of the liquid spray hole 8. Therefore, the ejected hydrogen can slow down the flow rate of the liquid high-purity sulfur ejected from the liquid spray hole 8, and the liquid high-purity sulfur is further diffused by the impact of the hydrogen, thereby increasing the contact area between the hydrogen and the liquid high-purity sulfur, further increasing the reaction rate, and accelerating the preparation efficiency of high-purity hydrogen sulfide. Initially, the electric push rod 22 is in a retracted state, pushing The rod 23 is in the center of the annular cylinder 9, and the lower end of the push rod 23 is not in contact with the sealing baffle 18. Therefore, under the action of the connecting spring 21, the sealing baffle 18 is in close contact with the lower surface of the diverter ring 6. Since the diameter of the sealing baffle 18 is smaller than the outer diameter of the diverter ring 6 and larger than the inner diameter of the diverter ring 6, the sealing baffle 18 can play a sealing role, so that hydrogen only exists in the space below the diverter ring 6, which is conducive to rapid filling of hydrogen and further allowing hydrogen to fully react with liquid high-purity sulfur; the first liquid sulfur pump is intermittently turned on according to the first preset time length, and can intermittently supply liquid to the diverter ring 6. After the first liquid sulfur pump stops supplying liquid, the electric push rod 22 is started, and the electric push rod 22 is driven The push rod 23 is driven to extend downward. When the lower end of the push rod 23 contacts the upper surface of the sealing baffle 18, the push rod 23 pushes the sealing baffle 18 to move downward, the connecting column 20 slides downward in the mounting hole 19, and the connecting spring 21 is stretched. At this time, a gap is generated between the sealing baffle 18 and the diverter ring 6, and the prepared high-purity hydrogen sulfide gas can flow upward through the gap between the sealing baffle 18 and the diverter ring 6. When the electric push rod 22 is extended to a preset length, the electric push rod 22 stops extending, and the air intake pump is turned off. The first collecting pump is started, and under the action of the first collecting pump, the high-purity hydrogen sulfide gas enters the hydrogen sulfide collecting assembly; the first collecting pump During the startup of the collecting pump, the first liquid sulfur pump and the air intake pump are both in the closed state, providing sufficient time for high-purity sulfur liquefaction and hydrogen heating. The first collecting pump automatically shuts down after being started for the second preset time, and then the electric push rod 22 drives the push rod 23 to retract to its original position. After the push rod 23 is fully retracted, the first liquid sulfur pump and the air intake pump are restarted. Under the action of the connecting spring 21, the connecting column 20 slides upward in the mounting hole 19, so that the upper surface of the sealing baffle 18 is re-attached to the lower surface of the diverter ring 6. Through the sealing effect of the sealing baffle 18, the liquid high-purity sulfur and hydrogen are fully reacted under the diverter ring 6 to produce high-purity hydrogen sulfide gas.

[0061] Example 8

[0062] On the basis of Example 7, Figure 3As shown, a first annular push plate 24 is provided in the liquid inlet chamber 12, and the outer wall of the first annular push plate 24 is connected to the inner wall of the liquid inlet chamber 12 for sliding up and down. A second annular push plate 25 is provided below the first annular push plate 24, and the second annular push plate 25 is connected to the first annular push plate 24 through a return spring 26. The lower end of the liquid supply pipe 15 passes through the first annular push plate 24 and is connected to the space between the first annular push plate 24 and the second annular push plate 25. An annular push block 27 is provided in the mixing chamber 13, and the outer wall of the annular push block 27 is connected to the inner wall of the mixing chamber 13 for sliding up and down. A movable disk 28 is provided outside the push rod 23, and a plurality of first push rods 29 and second push rods 30 are provided on the lower surface of the movable disk 28. The lower end of the first push rod 29 is connected to the upper surface of the first annular push plate 24, and the lower end of the second push rod 30 is connected to the upper surface of the annular push block 27.

[0063] The working principle and beneficial effects of the above technical solution are as follows: liquid high-purity sulfur is injected between the first annular push plate 24 and the second annular push plate 25 through the liquid supply pipe 15, and at the same time the air intake pump is started to transport hydrogen into the air cavity, and the hydrogen is sprayed into the reaction tower 2 from the nozzle 17, and flows into the mixing chamber 13 through the liquid spray hole 8, the annular cavity 7, and the delivery pipe 14. As the liquid high-purity sulfur increases, the second annular push plate 25 gradually slides toward the connecting hole, and the return spring 26 is stretched. When the first liquid sulfur pump stops supplying liquid, the second annular baffle is above the connecting hole, and then the electric push rod 22 is started and drives the push rod 23 to extend downward, and the push rod 23 drives the movable plate 28 to move downward, and the movable plate drives the first push rod 29 and the second push rod 30 to slide downward synchronously, and the movable plate 28 drives the first annular push plate 24 to slide downward through the lower end of the first push rod 29, and the first annular push plate 24 pushes the second annular push plate 25 to slide downward through the liquid high-purity sulfur. When the lower end of the second annular push plate 25 is aligned with the annular When the bottom wall of the cylinder 9 is in contact, as the first push rod 29 continues to push, the first annular push plate 24 slides toward the second annular push plate 25, thereby quickly squeezing the liquid high-purity sulfur between the first annular push plate 24 and the second annular push plate 25 into the mixing chamber 13. The liquid high-purity sulfur entering the mixing chamber 13 is preliminarily mixed and reacted with the hydrogen in the mixing chamber 13. At the same time, the second push rod 30 pushes the annular push block 27 to slide downward along the mixing chamber 13. Under the squeezing of the annular push block 27, the mixing chamber 13 is The liquid high-purity sulfur and hydrogen in the mixing chamber 13 flow rapidly through the delivery pipe 14 to the annular cavity 7 and out of the liquid spray hole 8. The hydrogen in the mixing chamber 13 increases in pressure under the push of the annular push block 27. Under the action of the high-pressure hydrogen, the liquid high-purity sulfur sprayed from the liquid spray hole 8 can be further diffused. Combined with the hydrogen sprayed from the nozzle 17, the contact area between the hydrogen and the liquid high-purity sulfur is further expanded, allowing the hydrogen and liquid high-purity sulfur to fully react, thereby improving the production efficiency of high-purity hydrogen sulfide.During the start-up process of the first liquid sulfur pump, the hydrogen below the diverter ring 6 can enter the mixing chamber 13 through the liquid spray hole 8. During the flow of hydrogen, the liquid spray hole 8, the annular cavity 7 and the inner wall of the delivery pipe 14 can be quickly impacted to remove the residual liquid high-purity sulfur, thereby preventing the liquid high-purity sulfur from remaining on the inner wall and solidifying to block the liquid spray hole 8 and the delivery pipe 14, thereby extending the service life of the device. The actual injection amount of liquid high-purity sulfur between the first annular push plate 24 and the second annular push plate 25 can be calculated based on the first preset time of the start-up of the first liquid sulfur pump and the flow rate in the liquid supply pipe 15. The target amount of hydrogen required for the reaction can be calculated based on the actual injection amount of liquid high-purity sulfur. The start-up time of the air intake pump is the first preset time of the start-up of the first liquid sulfur pump and the electric The time required for the push rod 22 to extend to a preset length is then calculated. The target flow rate of hydrogen gas can then be accurately calculated based on the target hydrogen flow rate and the duration the air intake pump is turned on. Finally, the output flow rate of the air intake pump can be adjusted based on the target hydrogen flow rate, thereby achieving precise control of the hydrogen amount. This, on the one hand, avoids waste caused by excessive hydrogen, and on the other hand, avoids incomplete reaction of liquid high-purity sulfur due to insufficient hydrogen, thereby ensuring a more complete reaction of hydrogen and liquid high-purity sulfur within the reaction tower 2. The periodic intermittent activation of the first liquid sulfur pump and the air intake pump not only avoids their continuous operation, reduces fatigue and extends their service life, but also reduces production energy consumption, achieving energy-saving effects and contributing to cost reduction and efficiency improvement for enterprises.

[0064] Example 9

[0065] On the basis of Example 8, Figure 3-Figure 6 As shown, a sliding groove 31 is provided on the inner wall of the annular cylinder 9, and one side of the sliding groove 31 is connected to the liquid inlet chamber 12. A sliding plate 32 is slidingly provided in the sliding groove 31, and the sliding plate 32 is connected to the inner wall of the sliding groove 31 through a number of compression springs 34. The sliding plate 32 is provided with a first vertical section, a connecting section and a second vertical section in sequence from top to bottom. The lower end of the first vertical section is connected to the second vertical section through the connecting section. The thickness of the upper end of the connecting section is the same as the thickness of the lower end of the first vertical section, and the thickness of the lower end of the connecting section is the same as the thickness of the upper end of the second vertical section. The thickness of the first vertical section is greater than the thickness of the second vertical section. A first guide slope is provided on the side of the connecting section close to the communicating hole, a stop block 33 is provided at the lower end of the second vertical section, and a second guide slope is provided on the side of the stop block 33 close to the communicating hole.

[0066] The working principle and beneficial effects of the above technical solution are as follows: a plurality of through holes are provided in the second annular push plate 25, and the through holes pass through the upper and lower surfaces of the second annular push plate 25. A second one-way valve is provided in the through hole, which can ensure that the liquid flows from the bottom of the second annular push plate 25 to the upper surface of the second annular push plate 25. When the second annular push plate 25 slides to the second vertical section and the first annular push plate 24 is in the first vertical section, part of the liquid high-purity sulfur can flow to the bottom of the second annular push plate 25 through the gap between the second annular push plate 25 and the second vertical section. When the first annular push plate 24 and the second annular push plate 25 both slide to the second vertical section of the sliding plate 32, under the action of the compression spring 34, the second vertical section contacts the first annular push plate 24 and the second annular push plate 25. As the first push rod 29 continues to push, the second annular push plate 25 slides along the second guide inclined surface and passes through the stop block 33 to contact the bottom wall of the liquid inlet chamber 12. In this process, the liquid high-purity sulfur below the second annular push plate 25 can flow upward along the through hole. The first annular push plate 24 is pushed downward by the first push plate 24 to squeeze the liquid high-purity sulfur out of the connecting hole. When the electric push rod 22 retracts, the first push rod 29 first drives the first annular push plate 24 to slide upward, and then pulls the second annular push plate 25 to slide upward by the return spring 26, but the lower end of the stopper 33 blocks the second annular push plate 25, so that the second annular push plate 25 slides upward until the first annular push plate 24 slides upward along the first guide inclined surface of the connecting section to the first vertical section, and the sliding plate 32 returns to its original position. Under the action of the return spring 26, the second annular push plate 25 slides upward quickly. Through the contact between the second annular push plate 25 and the inner wall of the liquid inlet chamber 12, the second annular push plate 25 scrapes and cleans the inner wall of the liquid inlet chamber 12 to prevent the connecting hole from being blocked by liquid high-purity sulfur, thereby extending the service life of the device.

[0067] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0068] In the present invention, unless otherwise specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection, or communication; direct connection or indirect connection through an intermediate medium; internal communication between two elements or interaction between two elements, unless otherwise specified. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0069] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the description and implementation methods. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and illustrations shown and described herein.

Claims

1. A device for preparing high-purity hydrogen sulfide, characterized in that: The invention comprises a sulfur melting kettle (1), a reaction tower (2) and a heater (3), wherein the output end of the sulfur melting kettle (1) is connected to the reaction tower (2) via a liquid inlet pipe, and a first liquid sulfur pump is provided on the liquid inlet pipe; the output end of the heater (3) is connected to the reaction tower (2) via an air inlet pipe, and an air inlet pump is provided on the air inlet pipe; A diverter ring (6) is provided in the reaction tower (2). The diverter ring (6) has an annular structure. The outer wall of the diverter ring (6) is connected to the inner wall of the reaction tower (2). An annular cavity (7) is provided in the diverter ring (6). A plurality of liquid spray holes (8) are provided at the bottom of the diverter ring (6). The upper ends of the liquid spray holes (8) are connected to the annular cavity (7). An annular cylinder (9) is provided above the diverter ring (6). The outer wall of the annular cylinder (9) is connected to the inner wall of the reaction tower (2) through a connecting plate (10). A separating ring (11) is provided in the annular cylinder (9). The central axis of the separating ring (11) is on the same straight line as the central axis of the annular cylinder (9). The separating ring (11) connects the annular cylinder ( 9) is divided into a liquid inlet chamber (12) and a mixing chamber (13), the mixing chamber (13) is located on the inner side of the separation ring (11), a plurality of communication holes are provided at the lower position of the separation ring (11), a one-way valve is provided in the communication hole, the liquid inlet chamber (12) is communicated with the mixing chamber (13) through the communication hole, a delivery hole is provided at the bottom of the mixing chamber (13), a delivery pipe (14) is provided at the lower end of the delivery hole, the delivery pipe (14) is communicated with the annular cavity (7) at one end away from the annular cylinder (9), a liquid supply pipe (15) is provided at the upper end of the annular cylinder (9), one end of the liquid supply pipe (15) is communicated with the liquid inlet chamber (12), and the other end of the liquid supply pipe (15) is connected to the liquid inlet pipe; A diverter disk (16) is provided below the diverter ring (6), an air cavity is provided in the diverter disk (16), an air inlet pipe is connected to the air cavity through an air supply pipe, a plurality of nozzles (17) are provided on the periphery of the diverter disk (16), one end of the nozzle (17) is connected to the air cavity, a sealing baffle (18) is provided on the top of the diverter disk (16), the sealing baffle (18) is connected to the diverter ring (6) through a connecting mechanism, the connecting mechanism includes a plurality of mounting holes (19) provided inside the diverter disk (16), a connecting column (20) is slidably provided in the mounting hole (19), the connecting column (20) is connected to the top wall of the mounting hole (19) through a connecting spring (21), the lower end of the connecting column (20) is connected to the upper surface of the sealing baffle (18), an electric push rod (22) is provided on the top of the reaction tower (2), a push rod (23) is provided at the output end of the electric push rod (22), and the lower end of the push rod (23) extends to the center of the annular cylinder (9).

2. The device for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: A stirring mechanism is provided in the molten sulfur kettle (1).

3. The device for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: A liquid return pipe is provided at the bottom of the reaction tower (2), one end of the liquid return pipe away from the reaction tower (2) is connected to the sulfur melting kettle (1), and a second liquid sulfur pump is provided on the liquid return pipe.

4. The device for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: The invention also includes a hydrogen sulfide collection component, which includes a condensation tank (4) and a hydrogen sulfide collection cylinder (5). Three condensation tanks (4) are provided. A condensation mechanism is provided in the condensation tank (4). Two adjacent condensation tanks (4) are connected by a connecting pipe. The inlet of the condensation tank (4) close to the reaction tower (2) is connected to the top of the reaction tower (2) through a first collection pipe. A first collection pump is provided on the first collection pipe. A discharge pipe is provided at the bottom of the condensation tank (4). The lower end of the discharge pipe is connected to the second collection pipe. The output end of the second collection pipe is connected to the hydrogen sulfide collection cylinder (5). A second collection pump is provided near the output end of the second collection pipe.

5. The device for preparing high-purity hydrogen sulfide according to claim 4, characterized in that: The outlet of the condensation tank (4) away from the reaction tower (2) is connected to the input end of the heater (3) through a hydrogen recovery pipe, and a hydrogen recovery pump is provided on the hydrogen recovery pipe.

6. The device for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: The upper end of the liquid spray hole (8) is funnel-shaped.

7. A process for preparing high-purity hydrogen sulfide, comprising: include: Obtaining high-purity sulfur, adding the high-purity sulfur into a sulfur melting kettle (1) for melting to obtain liquid high-purity sulfur; preparing hydrogen and heating the hydrogen; Liquid high-purity sulfur and heated hydrogen are sent to a reaction tower (2) for reaction to produce high-purity hydrogen sulfide gas.

8. The process for preparing high-purity hydrogen sulfide according to claim 7, characterized in that: High-purity sulfur is in granular or powder form.

9. The process for preparing high-purity hydrogen sulfide according to claim 7, characterized in that: The purity of hydrogen is greater than or equal to 99.9%.

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