Preparation process and preparation device of high-purity hydrogen sulfide

Abstract

The invention provides a preparation process and a preparation device of high-purity hydrogen sulfide, and relates to the technical field of hydrogen sulfide preparation, and the preparation process comprises the following steps: obtaining high-purity sulfur, adding the high-purity sulfur into a sulfur melting kettle, and melting to obtain liquid high-purity sulfur; hydrogen is prepared and heated; and feeding the liquid high-purity sulfur and the heated hydrogen into a reaction tower for reaction to prepare the high-purity hydrogen sulfide gas. According to the invention, hydrogen sulfide is prepared from high-purity sulfur and high-purity hydrogen, so that the generation of impurity gases can be reduced, and the purity of hydrogen sulfide gas is improved.

Description

Technical Field

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

[0002] Mercapto compounds are a class of organic compounds containing a mercapto (-SH) functional group, and mercapto compounds have a wide range of applications in multiple fields. In the preparation process of mercapto compounds, hydrogen sulfide can be introduced as a sulfur source into the mercapto group. To ensure the yield of mercapto compounds, a large amount of high-purity hydrogen sulfide is required in the preparation process.

[0003] Chinese Patent with the authorization announcement number CN115535967B discloses a method for preparing hydrogen sulfide, and the method includes: 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. No sodium ions will be introduced into the reaction system, and the post-treatment is relatively easy. Moreover, the natural mineral containing pyrrhotite is low in price and widely available, and is often associated with heavy non-ferrous metals such as copper, lead, and zinc. Therefore, it is easy to obtain during the copper, lead, and zinc ore dressing process, realizing the comprehensive utilization of resources, reducing the overall production cost, and the finally prepared hydrogen sulfide can be used for removing heavy metals in the wastewater or the sewage system during non-ferrous metal smelting. The method provided by the present invention is particularly suitable for use in non-ferrous metallurgy 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 power-free stirring.

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

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

[0006] To solve the above technical problem, the present invention discloses a preparation process for high-purity hydrogen sulfide, including:

[0007] Obtain high-purity sulfur, add the high-purity sulfur to a sulfur melting kettle for melting to obtain liquid high-purity sulfur;

[0008] Prepare hydrogen and heat the hydrogen;

[0009] Send the liquid high-purity sulfur and the heated hydrogen to a reaction tower for reaction to obtain high-purity hydrogen sulfide gas.

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

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

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

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

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

[0015] Preferably, it further includes a hydrogen sulfide collection assembly, which includes a condensation tank and a hydrogen sulfide collection steel cylinder. There are three condensation tanks, and a condensation mechanism is arranged in the condensation tank. Adjacent two condensation tanks are connected through 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 collection pipe, and a first collection pump is arranged on the first collection pipe. A drain pipe is arranged at the bottom of the condensation tank, and the lower end of the drain pipe is connected to a second collection pipe. The output end of the second collection pipe is connected to the hydrogen sulfide collection steel cylinder, and a second collection pump is arranged at a position close to the output end of the second collection pipe.

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

[0017] Preferably, a flow dividing ring is arranged in the reaction tower. The flow dividing ring is in a ring structure. The outer wall of the flow dividing ring is connected to the inner wall of the reaction tower. An annular cavity is arranged inside the flow dividing ring. A plurality of liquid spraying holes are arranged at the bottom of the flow dividing ring, and the upper ends of the liquid spraying holes are communicated with the annular cavity. An annular cylinder is arranged above the flow dividing ring. The outer wall of the annular cylinder is connected to the inner wall of the reaction tower through a connecting plate. A partition ring is arranged inside the annular cylinder. The central axis of the partition ring is on the same straight line as the central axis of the annular cylinder. The partition ring divides the inside of the annular cylinder into a liquid inlet chamber and a mixing chamber. The mixing chamber is located inside the partition ring. A plurality of communication holes are arranged at a position close to the lower part of the partition ring, and one-way valves are arranged in the communication holes. The liquid inlet chamber is communicated with the mixing chamber through the communication holes. A conveying hole is arranged at the bottom of the mixing chamber, and a conveying pipe is arranged at the lower end of the conveying hole. One end of the conveying pipe away from the annular cylinder is communicated with the annular cavity. A liquid supply pipe is arranged at the upper end of the annular cylinder. One end of the liquid supply pipe is communicated with 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 spraying hole is in a funnel shape.

[0019] The technical solution of the present invention has the following advantages: The present invention provides a preparation process and a preparation device for high-purity hydrogen sulfide, which relates to the technical field of hydrogen sulfide preparation. The process includes obtaining high-purity sulfur, adding the high-purity sulfur into a sulfur melting kettle for melting to obtain liquid high-purity sulfur; preparing hydrogen and heating the hydrogen; and sending the liquid high-purity sulfur and the heated hydrogen to a reaction tower for reaction to obtain high-purity hydrogen sulfide gas. In the present invention, high-purity sulfur and high-purity hydrogen are used to prepare hydrogen sulfide, which can reduce the generation of impurity gases and improve the purity of hydrogen sulfide gas.

[0020] Other features and advantages of the present invention will be described in the following specification, and, in part, will be obvious from the specification, or will be understood by implementing the present invention. The objectives and other advantages of the present invention can be achieved and obtained by the devices specifically pointed out in the written specification and the accompanying drawings of the specification.

[0021] The following will further describe in detail the technical solution of the present invention 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. They are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention. In the accompanying drawings:

[0023] Figure 1 is a process flow diagram of a preparation process for high-purity hydrogen sulfide according to the present invention;

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

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

[0026] Figure 4 For the present invention Figure 3 is an enlarged view of the structure at A in the present invention;

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

[0028] Figure 6 For the present invention Figure 5 is an enlarged view of the structure at B in the present invention;

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

[0030] In the figure: 1, sulfur melting kettle; 2, reaction tower; 3, heater; 4, condensation tank; 5, hydrogen sulfide collection steel cylinder; 6, shunt ring; 7, annular cavity; 8, liquid spraying hole; 9, annular cylinder; 10, connecting plate; 11, partition ring; 12, liquid inlet cavity; 13, mixing cavity; 14, conveying pipe; 15, liquid supply pipe; 16, shunt plate; 17, spray head; 18, sealing baffle; 19, mounting hole; 20, connecting column; 21, connecting spring; 22, electric push rod; 23, pushing rod; 24, first annular push plate; 25, second annular push plate; 26, reset spring; 27, annular push block; 28, moving plate; 29, first push rod; 30, second push rod; 31, sliding groove; 32, sliding plate; 33, stop block; 34, compression spring. Detailed implementation manners

[0031] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining 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 for descriptive purposes, and do not particularly refer to the meaning of 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 quantity of the indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In addition, the technical solutions and technical features between various embodiments can be combined with each other, but it must be based on the fact that those skilled in the art can implement them. When the combination of technical solutions appears to be contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0033] Embodiment 1

[0034] The embodiment of the present invention provides a preparation process of high-purity hydrogen sulfide, as Figure 1 shown, including:

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

[0036] Prepare hydrogen and heat the hydrogen;

[0037] Send the liquid high-purity sulfur and the heated hydrogen to the reaction tower 2 for reaction to obtain high-purity hydrogen sulfide gas;

[0038] The high-purity sulfur is in granular or powdery 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, with a purity of at least 99.9%. Then, the high-purity sulfur is added to the sulfur melting kettle 1 for melting to obtain liquid high-purity sulfur. Next, hydrogen is prepared, with a purity of not less than 99.9%, and the hydrogen is heated to prevent the temperature of the hydrogen introduced into the reaction tower 2 from being too low and affecting the reaction process. 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. The hydrogen sulfide gas produced is not likely to be mixed with impurity gases such as carbon dioxide and sulfur dioxide, reducing the generation of impurity gases, and no by-products such as iron-containing sulfates will be produced. Finally, high-purity hydrogen sulfide gas is obtained, improving the purity of the hydrogen sulfide gas, which is beneficial for large-scale industrial use.

[0041] Example 2

[0042] Based on the above Example 1, as Figures 2 - 7 shown, the embodiment of the present invention also provides a preparation device for high-purity hydrogen sulfide, including: a sulfur melting kettle 1, a reaction tower 2, and a heater 3. The output end of the sulfur melting 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. 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: When using the preparation device to prepare high-purity hydrogen sulfide, first add the prepared high-purity sulfur into the sulfur melting kettle 1, and keep the temperature in the sulfur melting kettle 1 at 300 - 500 °C to ensure that the high-purity sulfur is fully melted. At the same time, the prepared high-purity hydrogen is introduced into the heater 3 for preheating, and the preheating temperature can be set by the user. 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 introduced into the reaction tower 2 by the air inlet pump. The temperature in the reaction tower 2 is not lower than 300 °C, and the liquid high-purity sulfur and hydrogen react in the high-temperature environment of the reaction tower 2 to obtain hydrogen sulfide gas. During the preparation process, high-purity sulfur and high-purity hydrogen are used to prepare hydrogen sulfide. The hydrogen sulfide gas produced is not likely to be mixed with impurity gases such as carbon dioxide and sulfur dioxide, reducing the generation of impurity gases, and no by-products such as iron-containing sulfates will be produced. Finally, 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, making the reaction more complete.

[0044] Example 3

[0045] Based on Example 2, a stirring mechanism is provided inside the sulfur melting kettle 1.

[0046] The working principle and beneficial effects of the above technical solution are as follows: The stirring mechanism can stir the high-purity sulfur in the sulfur melting kettle 1, making the high-purity sulfur fully melted, improving the melting effect and melting efficiency.

[0047] Example 4

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

[0049] The working principle and beneficial effects of the above technical solution are as follows: The unreacted liquid high-purity sulfur flows to the bottom of the reaction tower 2. A liquid level monitoring device is arranged on the reaction tower 2, and the liquid level monitoring device is used to monitor the liquid level height of the liquid high-purity sulfur in the reaction tower 2. A controller is arranged 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 height of the liquid high-purity sulfur in the reaction tower 2 is higher than the preset liquid level height, the controller outside the reaction tower 2 controls the second liquid sulfur pump to start. Through the second liquid sulfur pump, the liquid high-purity sulfur in the reaction tower 2 can be pumped into the liquid return pipe and transported into the molten sulfur kettle 1 through the liquid return pipe, which is beneficial to the recycling of liquid high-purity sulfur. When the liquid level height 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 pumping out all the liquid high-purity sulfur and prevent the gas in the reaction tower 2 from entering the molten sulfur kettle 1.

[0050] Example 5

[0051] On the basis of any one of Examples 2-4, as Figure 2 shown, it further includes a hydrogen sulfide collection component. The hydrogen sulfide collection component includes three condensation tanks 4 and a hydrogen sulfide collection steel cylinder 5. A condensation mechanism is arranged in the condensation tank 4. Adjacent two condensation tanks 4 are connected through 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, and a first collection pump is arranged on the first collection pipe. A drain pipe is arranged at the bottom of the condensation tank 4, and the lower end of the drain pipe is connected to a second collection pipe. The output end of the second collection pipe is connected to the hydrogen sulfide collection steel cylinder 5, and a second collection pump is arranged at a position close to the output end of the second collection pipe;

[0052] The outlet of the condensation tank 4 far 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 arranged 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 there is still a small amount of unreacted hydrogen mixed in the high-purity hydrogen sulfide gas. Therefore, a hydrogen sulfide collection component is provided to collect the prepared high-purity hydrogen sulfide. Specifically, start the first collection pump, and the first collection pump can extract the gas in the reaction tower 2 to the first condensation tank 4 through the first collection pipe. The gas passes through the first condensation tank 4, the second condensation tank 4, and the third condensation tank 4 in sequence. The high-purity hydrogen sulfide gas in the gas is liquefied into hydrogen sulfide liquid and flows to the second collection pipe through the drain pipe. Open the second collection pump to extract the hydrogen sulfide liquid in the second collection pipe into the hydrogen sulfide collection steel cylinder 5 for collection. Finally, high-purity hydrogen sulfide liquid is collected. The mixed hydrogen passes through the third condensation tank 4 and then enters the hydrogen recovery pipe through the outlet of the condensation tank 4, and flows into the heater 3 under the action of the hydrogen recovery pump for heating. 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, achieving the effect of energy saving, reducing the preparation cost. A hydrogen inlet is also provided on the heater 3, and hydrogen can be introduced through the hydrogen inlet to ensure the amount of hydrogen required for production. A condensation mechanism is provided in the condensation tank 4. The condensation mechanism includes a spiral cooling pipe, and a cooling liquid flows in the spiral cooling pipe. The hydrogen sulfide gas passing by is cooled by continuously refrigerating and circulating the cooling liquid, reducing the temperature of the hydrogen sulfide gas, so that the hydrogen sulfide gas is gradually condensed into hydrogen sulfide liquid. The temperature in the first condensation tank 4 from left to right is maintained at -10°C to 0°C, the temperature in the second condensation tank 4 is maintained at -45°C to -35°C, and the temperature in the third condensation tank 4 is maintained at -85°C to -75°C. The hydrogen sulfide gas passing by is gradually cooled, so that the hydrogen sulfide gas is fully liquefied and finally collected into the hydrogen sulfide collection steel cylinder 5. The mixed hydrogen flows into the hydrogen recovery pipe in a gaseous form through the outlet of the third condensation tank 4, realizing the separation of hydrogen sulfide and hydrogen, and ensuring the purity of the hydrogen sulfide liquid in the hydrogen sulfide collection steel cylinder 5. There is hydrogen sulfide liquid remaining in the second collection pipe, which can prevent hydrogen from mixing into the hydrogen sulfide collection steel cylinder 5.

[0054] Example 6

[0055] On the basis of any one of Examples 2-5, if Figures 3 - 7As shown in the figure, a flow dividing ring 6 is arranged in the reaction tower 2. The flow dividing ring 6 is of a ring structure. The outer wall of the flow dividing ring 6 is connected to the inner wall of the reaction tower 2. An annular cavity 7 is arranged inside the flow dividing ring 6. A plurality of liquid spraying holes 8 are arranged at the bottom of the flow dividing ring 6. The upper end of the liquid spraying hole 8 is communicated with the annular cavity 7. An annular cylinder 9 is arranged above the flow dividing 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 dividing ring 11 is arranged inside the annular cylinder 9. The central axis of the dividing ring 11 is on the same straight line as the central axis of the annular cylinder 9. The dividing ring 11 divides the inside of the annular cylinder 9 into a liquid inlet cavity 12 and a mixing cavity 13. The mixing cavity 13 is located inside the dividing ring 11. A plurality of communicating holes are arranged at a lower position of the dividing ring 11. One-way valves are arranged in the communicating holes. The liquid inlet cavity 12 is communicated with the mixing cavity 13 through the communicating holes. A conveying hole is arranged at the bottom of the mixing cavity 13. A conveying pipe 14 is arranged at the lower end of the conveying hole. One end of the conveying pipe 14 away from the annular cylinder 9 is communicated with the annular cavity 7 of the flow dividing ring 6. A liquid supply pipe 15 is arranged at the upper end of the annular cylinder 9. One end of the liquid supply pipe 15 is communicated with the liquid inlet cavity 12. The other end of the liquid supply pipe 15 is connected to the liquid inlet pipe;

[0056] The upper end of the liquid spraying 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 is a telescopic pipe. The liquid high-purity sulfur flows into the liquid inlet cavity 12 through the liquid supply pipe 15, then enters the mixing cavity 13 through the communicating holes, and then is conveyed to the annular cavity 7 of the flow dividing ring 6 through the conveying pipe 14, and finally sprays downward through the liquid spraying holes 8. The flow dividing ring 6 can disperse and flow out the liquid high-purity sulfur, increasing the contact area between the liquid high-purity sulfur and hydrogen, facilitating the full reaction between the liquid high-purity sulfur and hydrogen in the reaction tower 2, improving the reaction rate, and the liquid droplets of the liquid high-purity sulfur can quickly diffuse in hydrogen, making the mixing of high-purity sulfur and hydrogen more uniform. A plurality of liquid spraying holes 8 are arranged. The plurality of liquid spraying holes 8 are arranged in an annular array at the bottom of the flow dividing ring 6. The liquid high-purity sulfur can flow out evenly through the plurality of liquid spraying holes 8. The upper end of the liquid spraying hole 8 is funnel-shaped, which can prevent the liquid high-purity sulfur from remaining in the liquid inlet cavity 12.

[0058] Example 7

[0059] On the basis of Example 6, as Figure 3As shown in the figure, a flow dividing disk 16 is arranged below the flow dividing ring 6. An air cavity is arranged inside the flow dividing disk 16. The intake pipe is communicated with the air cavity through a supply pipe. A plurality of nozzles 17 are arranged on the outer periphery of the flow dividing disk 16. One end of each nozzle 17 is communicated with the air cavity. A sealing baffle 18 is arranged on the top of the flow dividing disk 16. The sealing baffle 18 is connected with the flow dividing ring 6 through a connecting mechanism. The connecting mechanism includes a plurality of mounting holes 19 arranged inside the flow dividing disk 16. A connecting column 20 is slidably arranged inside the mounting hole 19. The connecting column 20 is connected with the top wall of the mounting hole 19 through a connecting spring 21. The lower end of the connecting column 20 is connected with the upper surface of the sealing baffle 18. An electric push rod 22 is arranged on the top of the reaction tower 2. A push rod 23 is arranged at the output end of the electric push rod 22. 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 improve the reaction rate, a flow dividing plate 16 is arranged below the flow dividing ring 6. Hydrogen enters the air cavity through a telescopic gas supply pipe and then is ejected through a plurality of nozzles 17. The direction of hydrogen ejected by the nozzles 17 intersects with the flow direction of the liquid ejection holes 8. Therefore, the ejected hydrogen can slow down the flow rate of the liquid high-purity sulfur ejected from the liquid ejection holes 8, and through the impact of hydrogen, the liquid high-purity sulfur is further diffused, increasing the contact area between hydrogen and liquid high-purity sulfur, further improving the reaction rate, and accelerating the preparation efficiency of high-purity hydrogen sulfide. Initially, the electric push rod 22 is in the retracted state, the push rod 23 is at the center of the annular cylinder 9, and the lower end of the push rod 23 does not contact the sealing baffle 18. Therefore, under the action of the connecting spring 21, the sealing baffle 18 is closely attached to the lower surface of the flow dividing ring 6. Since the diameter of the sealing baffle 18 is smaller than the outer diameter of the flow dividing ring 6 and larger than the inner diameter of the flow dividing ring 6, the sealing baffle 18 can play a sealing role, enabling hydrogen to exist only in the space below the flow dividing ring 6, which is beneficial for hydrogen to quickly fill up and further enables hydrogen to fully react with liquid high-purity sulfur; the first liquid sulfur pump is intermittently started according to the first preset duration and can supply liquid to the flow dividing ring 6 intermittently. After the first liquid sulfur pump stops supplying liquid, the electric push rod 22 is started. The electric push rod 22 drives the push rod 23 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, and 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 flow dividing ring 6, and the prepared high-purity hydrogen sulfide gas can flow upward through the gap between the sealing baffle 18 and the flow dividing ring 6. When the electric push rod 22 extends to the preset length, the electric push rod 22 stops extending, and at the same time, the air inlet pump is closed and the first collection pump is started. Under the action of the first collection pump, the high-purity hydrogen sulfide gas enters the hydrogen sulfide collection assembly; during the process of starting the first collection pump, both the first liquid sulfur pump and the air inlet pump are in the closed state, providing sufficient duration for the liquefaction of high-purity sulfur and the heating of hydrogen. After the first collection pump is started for the second preset duration, it is automatically closed, and then the electric push rod 22 drives the push rod 23 to retract to the original position. After the push rod 23 is completely retracted, the first liquid sulfur pump and the air inlet 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 reattached to the lower surface of the flow dividing ring 6. Through the sealing action of the sealing baffle 18, the liquid high-purity sulfur and hydrogen fully react below the flow dividing ring 6 to produce high-purity hydrogen sulfide gas.

[0061] Example 8

[0062] On the basis of Example 7, as Figure 3As shown in the figure, a first annular push plate 24 is arranged in the liquid inlet cavity 12. The outer wall of the first annular push plate 24 is slidably connected to the inner wall of the liquid inlet cavity 12 up and down. A second annular push plate 25 is arranged below the first annular push plate 24. 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 communicates with the space between the first annular push plate 24 and the second annular push plate 25. An annular push block 27 is arranged in the mixing cavity 13. The outer wall of the annular push block 27 is slidably connected to the inner wall of the mixing cavity 13 up and down. A moving disk 28 is arranged outside the push rod 23. A plurality of first push rods 29 and second push rods 30 are arranged on the lower surface of the moving disk 28. The lower end of the first push rod 29 is connected to the upper surface of the first annular push plate 24. 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 injection 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 reset 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 moving plate 28 to move downward, and the moving plate drives the first push rod 29 and the second push rod 30 to slide downward synchronously, and the moving 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 push plate 26, the moving plate 28 drives the first annular push plate 24 to slide downward. When the first push rod 29 contacts the bottom wall of the cylinder 9, as the first push rod 29 continues to push, the first annular push plate 24 slides toward the second annular push plate 25, so that the liquid high-purity sulfur between the first annular push plate 24 and the second annular push plate 25 is quickly squeezed into the mixing chamber 13, and 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 quickly flow to the annular cavity 7 through the delivery pipe 14 and flow out from the liquid spray hole 8. The hydrogen in the mixing chamber 13 increases its pressure under the push of the annular push block 27. Under the action of the relatively high-pressure hydrogen, the liquid high-purity sulfur sprayed from the liquid spray hole 8 can be more 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, so that the hydrogen and the liquid high-purity sulfur react fully, thereby improving the preparation efficiency of high-purity hydrogen sulfide.During the startup process of the first liquid sulfur pump, the hydrogen gas below the shunt ring 6 can enter the mixing chamber 13 through the liquid injection holes 8. During the flow of the hydrogen gas, it can rapidly impact the inner walls of the liquid injection holes 8, the annular cavity 7, and the delivery pipe 14, clearing the residual liquid high-purity sulfur, preventing the residual liquid high-purity sulfur from solidifying on the inner walls and blocking the liquid injection holes 8 and the delivery pipe 14, thus extending the service life of the device. The actual injection volume of the 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 duration of the startup of the first liquid sulfur pump and the flow rate in the supply pipe 15. Based on the actual injection volume of the liquid high-purity sulfur, the target amount of hydrogen gas required for the reaction can be calculated. The startup duration of the intake pump is the sum of the first preset duration of the startup of the first liquid sulfur pump and the duration required for the electric push rod 22 to extend to the preset length. Then, based on the target amount of hydrogen gas and the startup duration of the intake pump, the target flow rate of the hydrogen gas introduced can be accurately calculated. Finally, based on the target flow rate of the hydrogen gas introduced, the output flow rate of the intake pump can be adjusted, thereby achieving precise control of the hydrogen gas volume. On the one hand, it avoids waste caused by excessive hydrogen gas, and on the other hand, it avoids incomplete reaction of the liquid high-purity sulfur due to insufficient hydrogen gas, making the reaction between the hydrogen gas and the liquid high-purity sulfur in the reaction tower 2 more complete. The periodic intermittent startup of the first liquid sulfur pump and the intake pump can not only prevent the first liquid sulfur pump and the intake pump from running continuously, reduce the fatigue degree of the first liquid sulfur pump and the intake pump, and extend the service life, but also reduce the preparation energy consumption, achieving an energy-saving effect and contributing to the cost reduction and efficiency improvement of the enterprise.

[0064] Example 9

[0065] On the basis of Example 8, as Figures 3 - 6 shown, a sliding groove 31 is provided on the inner wall of the annular cylinder 9. One side of the sliding groove 31 is communicated with the liquid inlet chamber 12. A sliding plate 32 is slidably arranged in the sliding groove 31. The sliding plate 32 is connected to the inner wall of the sliding groove 31 through a plurality of compression springs 34. The sliding plate 32 is sequentially provided with a first vertical section, a connecting section, and a second vertical section 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 guiding inclined surface is provided on the connecting section close to the communication hole, and a stop block 33 is provided at the lower end of the second vertical section. A second guiding inclined surface is provided on the stop block 33 close to the communication hole.

[0066] The working principle and beneficial effects of the above technical solution are as follows: A number of through holes are provided in the second annular push plate 25, which penetrate the upper and lower surfaces of the second annular push plate 25. Second one-way valves are provided in the through holes, 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 while the first annular push plate 24 is in the first vertical section, part of the liquid high-purity sulfur can flow to the lower part of the second annular push plate 25 through the gap between the second annular push plate 25 and the second vertical section. When both the first annular push plate 24 and the second annular push plate 25 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. With the continuous push of the first push rod 29, the second annular push plate 25 slides along the second guiding inclined plane and contacts the bottom wall of the liquid inlet cavity 12 after passing through the stop block 33. During this process, the liquid high-purity sulfur located below the second annular push plate 25 can flow upward along the through holes, thereby pushing the liquid high-purity sulfur upward. The liquid high-purity sulfur flows between the first annular push plate 24 and the second annular push plate 25 through the impact force, reducing the phenomenon that part of the liquid high-purity sulfur solidifies during the conveying process. Finally, the first annular push plate 24 pushes downward to extrude the liquid high-purity sulfur from the communication 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 through the return spring 26. However, the lower end of the stop block 33 blocks the second annular push plate 25, causing the second annular push plate 25 to slide upward until the first annular push plate 24 slides upward along the first guiding inclined plane of the connecting section to the first vertical section, and then 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 rapidly. Through the contact between the second annular push plate 25 and the inner wall of the liquid inlet cavity 12, the second annular push plate 25 scrapes and cleans the inner wall of the liquid inlet cavity 12, preventing the communication hole from being bonded and blocked by the liquid high-purity sulfur, and extending the service life of the device.

[0067] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. are based on the orientation or positional relationship shown in the drawings. It is 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 construed as a limitation to the present invention.

[0068] In the present invention, unless otherwise clearly defined and limited, terms such as "installed", "connected", "linked", "fixed", etc. shall be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or integrated; it may be a mechanical connection, an electrical connection, or capable of communicating with each other; it may be directly connected, or indirectly connected through an intermediate medium, and may be the communication inside two elements or the interaction relationship between two elements, unless otherwise clearly defined. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0069] Although the embodiments of the present invention have been disclosed as above, it is not limited to the applications listed in the specification and embodiments. It can be fully applied to various fields suitable for the present invention. For those familiar with the field, additional modifications can be easily made. Therefore, without departing from the general concept defined by the claims and the equivalent scope, the present invention is not limited to the specific details and the illustrated and described examples here.

Claims

1. A process for preparing high-purity hydrogen sulfide, characterized in that: include: Obtaining high-purity sulfur, adding the high-purity sulfur into a sulfur melting kettle (1) for melting, and obtaining 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.

2. A process for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: High purity sulfur is in granular or powder form.

3. A process for preparing high-purity hydrogen sulfide according to claim 1, characterized in that: The purity of hydrogen is greater than or equal to 99.9%.

4. A device for preparing high-purity hydrogen sulfide, which uses a process for preparing high-purity hydrogen sulfide as described in any one of claims 1 to 3 to prepare high-purity hydrogen sulfide, characterized in that: The invention comprises 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) via a liquid inlet pipe, a first liquid sulfur pump is arranged on the liquid inlet pipe, and the output end of the heater (3) is connected to the reaction tower (2) via an air inlet pipe, an air inlet pump is arranged on the air inlet pipe.

5. A device for preparing high-purity hydrogen sulfide according to claim 4, characterized in that: A stirring mechanism is arranged in the molten sulfur kettle (1).

6. A device for preparing high-purity hydrogen sulfide according to claim 4, characterized in that: A liquid return pipe is arranged 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 molten sulfur kettle (1), and a second liquid sulfur pump is arranged on the liquid return pipe.

7. A device for preparing high-purity hydrogen sulfide according to claim 4, characterized in that: The invention also comprises a hydrogen sulfide collection component, which comprises 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 tanks (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.

8. The device for preparing high-purity hydrogen sulfide according to claim 7, characterized in that: The outlet of the condensation tank (4) far 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 arranged on the hydrogen recovery pipe.

9. The device for preparing high-purity hydrogen sulfide according to claim 4, characterized in that: A diverter ring (6) is arranged 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 arranged in the diverter ring (6). A plurality of liquid spray holes (8) are arranged 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 arranged 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 arranged in the annular cylinder (9). The central axis of the separator ring (11) is on the same straight line as the central axis of the annular cylinder (9). The separator ring (11) connects the annular cylinder (9) to the inner wall of the reaction tower (2). 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 dividing ring (11). A plurality of connecting holes are arranged at the lower position of the dividing ring (11). One-way valves are arranged in the connecting holes. The liquid inlet chamber (12) is connected with the mixing chamber (13) through the connecting holes. A delivery hole is arranged at the bottom of the mixing chamber (13). A delivery pipe (14) is arranged at the lower end of the delivery hole. The end of the delivery pipe (14) away from the annular cylinder (9) is connected with the annular cavity (7). A liquid supply pipe (15) is arranged at the upper end of the annular cylinder (9). One end of the liquid supply pipe (15) is connected with the liquid inlet chamber (12), and the other end of the liquid supply pipe (15) is connected with the liquid inlet pipe.

10. The device for preparing high-purity hydrogen sulfide according to claim 9, characterized in that: The upper end of the liquid spray hole (8) is funnel-shaped.

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