Hydrogenation reduction reaction tube for high-purity phosphorus
By setting up baffle and reaction pores in the hydrogenation reaction tube of high -pure phosphorus, increase the stay time and gas dispersal of the reactant, solve the problem of insufficient raw material response, and realize the improvement of phosphorus steam production and improvement of production efficiency. At the same time, production safety is enhanced.
Patent Information
- Application Number
- CN202420810053.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-18
- Publication Date
- 2025-01-28
- Estimated Expiration
- 2034-04-18
AI Technical Summary
In the existing high-purity phosphorus hydrogenation reduction reaction tubes, the raw material reaction is insufficient, resulting in insufficient production of phosphorus vapor, low production efficiency, and safety hazards.
The hydrogenation reaction tube of high -purity phosphorus is designed. By setting up a baffle in the reaction cavity, the reaction area and the collection area are divided along the axis direction to increase the residence time of the reactor in the tube, and the gas is more dispersed through the reaction hole. Make the reaction more.
Increased the output of phosphorus steam, improved production efficiency, reduced residual production raw materials, and improved production safety.
Smart Images
Figure CN222401486U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical equipment, in particular to a high-purity phosphorus hydrogenation reduction reaction tube. Background Art
[0002] High-purity phosphorus usually refers to elemental phosphorus containing 99.9999% (6N) phosphorus in the product. Elemental phosphorus above 6N is an important raw material for the production of electronic-grade red phosphorus and phosphorus compounds, such as chlorinated phosphorus and electronic-grade phosphoric acid. The existing high-purity phosphorus collection is done by injecting raw materials phosphorus trichloride and hydrogen into the reaction tube, heating the reaction tube with a heater, and reaching the temperature to produce phosphorus vapor and hydrochloric acid gas by hydrogenation reduction reaction. The phosphorus vapor is discharged at the outlet into the collection tower, but the reaction of the raw materials in the existing reaction tube is not sufficient, resulting in insufficient phosphorus vapor production and low production efficiency. At the same time, since phosphorus trichloride is toxic and hydrogen is flammable and explosive. If the unreacted phosphorus trichloride and hydrogen accumulate to a certain extent, it may pose a safety hazard. Utility Model Content
[0003] The utility model aims to solve at least one of the technical problems existing in the prior art. The utility model provides a high-purity phosphorus hydrogenation reduction reaction tube, which makes the raw material reaction more complete, increases the output of phosphorus vapor, improves production efficiency, and improves production safety.
[0004] In order to achieve the above-mentioned purpose, the utility model provides a high-purity phosphorus hydrogenation reduction reaction tube, comprising a main body, a baffle and a heating element for heating the main body, the main body is provided with a collecting port, a raw material filling port and a reaction chamber, the baffle is located in the reaction chamber and connected to the inner wall of the main body, the baffle is provided with a reaction through hole, the baffle is divided into a reaction zone and a collecting zone in the reaction chamber, the raw material filling port is connected to the reaction zone, the reaction zone is connected to the collecting zone through the reaction through hole, and the collecting zone is connected to the collecting port.
[0005] As a preferred solution, the reaction through hole is arranged on the upper part of the baffle.
[0006] As a preferred solution, the collecting port and the raw material filling port are respectively located at two ends of the main pipe body, and the baffle is located between the collecting port and the raw material filling port in the axial direction of the main pipe body.
[0007] As a preferred embodiment, it also includes an inner tube body, which includes a first inner tube body and a second inner tube body, one end of the first inner tube body is connected to the baffle, and the other end has a first flow gap with the end of the main tube body away from the collecting port, the second inner tube body is connected to the end of the main tube body away from the collecting port, one end of the second inner tube body extends into the first inner tube body and has a second flow gap with the baffle, and the other end extends out of the main tube body and is connected to the raw material filling port.
[0008] As a preferred solution, all of the reaction through holes are arranged between the outer wall of the first inner tube body and the inner wall of the main tube body.
[0009] As a preferred solution, the inner tube body further comprises a first connecting portion, one end of which is connected to the outer wall of the second inner tube body, and the other end of which is connected to the inner wall of the first inner tube body.
[0010] As a preferred solution, the inner tube body further comprises a second connecting portion, one end of which is connected to the outer wall of the first inner tube body, and the other end of which is connected to the inner wall of the main tube body.
[0011] As a preferred solution, the raw material filling port includes a gas filling port and a liquid filling port, and the liquid filling port and the gas filling port are respectively connected to an end of the second inner tube body away from the first inner tube body.
[0012] As a preferred solution, the axial distance between the liquid filling port and the baffle is a, and the axial distance between the gas filling port and the baffle is b, and b>a.
[0013] As a preferred solution, the collecting port is located below the filling port, the collecting port is located outside the heating element, and the main pipe is arranged to be inclined as a whole.
[0014] Compared with the prior art, the utility model embodiment of a high-purity phosphorus hydrogenation reduction reaction tube has the following beneficial effects: the heating element heats the main body to make the raw material reach the reaction temperature. The reaction chamber is divided into a reaction zone and a collection zone along the axial direction by a baffle, and the reaction zone is connected to the raw material filling port. The raw materials phosphorus trichloride and hydrogen enter the reaction zone through the raw material filling port and react in the reaction zone. Under the action of the baffle, the reactants are blocked when flowing out toward the collection zone, increasing the residence time of the reactants in the tube, and at the same time, the gas is more dispersed, so that the reaction is more complete, thereby increasing the output of phosphorus vapor, improving production efficiency, reducing residual production raw materials, and improving production safety. After the phosphorus trichloride is gasified, it enters the collection zone through the reaction through hole and is discharged from the collection port to realize the collection of the product phosphorus vapor. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 It is a schematic diagram of the overall structure of an embodiment of the utility model.
[0016] Figure 2 It is a cross-sectional view of the overall structure of an embodiment of the utility model.
[0017] Figure 3 This utility model embodiment Figure 1 Schematic diagram of the structure of the baffle at CC in FIG.
[0018] Figure 4 It is a schematic diagram of the flow path of the reactants in the main tube, the first inner tube and the second inner tube in an embodiment of the utility model.
[0019] Figure 5 This utility model embodiment Figure 2 Schematic diagram of the enlarged structure at D in FIG.
[0020] In the figure:
[0021] 10. Main body; 11. Collection port; 12. Raw material filling port; 13. Gas filling port; 14. Liquid filling port; 15. Reaction chamber; 16. Reaction zone; 17. Collection zone;
[0022] 20. baffle; 21. reaction through hole;
[0023] 30. Heating element;
[0024] 40. first inner tube body; 41. first flow gap; 42. second connecting portion;
[0025] 50. Second inner tube body; 51. Second flow gap; 52. First connecting portion. DETAILED DESCRIPTION
[0026] The following is a further detailed description of the specific implementation of the present invention in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
[0027] In the description of the present invention, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like used in the present invention to indicate the orientation or position relationship are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.
[0028] In the description of the present invention, it should be understood that the terms "connected", "connected", "fixed" and the like used in the present invention should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, or a welding connection; it can be directly connected, or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0029] like Figures 1 to 5 As shown, a high-purity phosphorus hydrogenation reduction reaction tube according to a preferred embodiment of the utility model comprises a main body 10, a baffle 20 and a heating element 30 for heating the main body 10, the main body 10 is provided with a collecting port 11, a raw material filling port 12 and a reaction chamber 15, the baffle 20 is located in the reaction chamber 15 and connected to the inner wall of the main body 10, the baffle 20 is provided with a reaction through hole 21, the baffle 20 divides the reaction chamber 15 into a reaction zone 16 and a collecting zone 17, the raw material filling port 12 is connected to the reaction zone 16, the reaction zone 16 is connected to the collecting zone 17 through the reaction through hole 21, and the collecting zone 17 is connected to the collecting port 11.
[0030] In the high-purity phosphorus hydrogenation reduction reaction tube of the utility model, the heating element 30 heats the main body 10 so that the raw material reaches the reaction temperature. The reaction chamber 15 is divided into a reaction zone 16 and a collection zone 17 along the axial direction by a baffle 20. The reaction zone 16 is connected to the raw material filling port 12. The raw materials phosphorus trichloride and hydrogen enter the reaction zone 16 through the raw material filling port 12, and react in the reaction zone 16. Under the action of the baffle 20, the reactant is blocked when flowing out toward the collection zone 17, which increases the residence time of the reactant in the tube, and at the same time, the gas is more dispersed, so that the reaction is more complete, thereby increasing the output of phosphorus vapor, improving production efficiency, reducing residual production raw materials, and improving production safety. After the phosphorus trichloride is gasified, it enters the collection zone 17 through the reaction through hole 21 and is discharged from the collection port 11, so that the product phosphorus vapor is collected.
[0031] As one embodiment, the chemical reaction formula in the main body 10 is: 2PCl3+3H2→2P+6HCl, and the gaseous phosphorus and gaseous hydrochloric acid are discharged and collected through the collection port 11.
[0032] Further, such as Figures 2 to 3 As shown, the reaction through hole 21 is arranged on the upper part of the baffle 20. Since the reaction tube is mainly used to reduce phosphorus trichloride to obtain phosphorus vapor, the specific gravity of gasified phosphorus trichloride is heavier than hydrogen, and most of it will be deposited under the main body 10. The reaction through hole 21 is arranged on the upper part of the baffle 20 to block the outflow of phosphorus trichloride gas and make the reaction more complete.
[0033] As one embodiment, Figures 2 to 3 As shown, a plurality of reaction through holes 21 are provided, and the plurality of reaction through holes 21 are all located at the upper portion of the baffle 20 , so that the gas can be dispersed more evenly and the reaction can be more complete.
[0034] Further, such as Figures 2 to 3As shown, the collecting port 11 and the filling port 12 are respectively located at the two ends of the main pipe body 10, and the baffle 20 is located between the collecting port 11 and the raw material filling port 12 in the axial direction of the main pipe body 10, extending the distance between the collecting port 11 and the raw material filling port 12, extending the wandering path of the reactants in the pipe, and making the reaction more complete.
[0035] Further, such as Figures 4 to 5 As shown, the inner tube body is also included, and the inner tube body includes a first inner tube body 40 and a second inner tube body 50. One end of the first inner tube body 40 is connected to the baffle 20, and the other end has a first flow gap 41 with the end of the main tube body 10 away from the collecting port 11. The second inner tube body 50 is connected to the end of the main tube body 10 away from the collecting port 11. One end of the second inner tube body 50 extends into the first inner tube body 40 and has a second flow gap 51 with the baffle 20, and the other end extends out of the main tube body 10 and communicates with the raw material filling port 12. The first inner tube body 40 and the second inner tube body 50 extend axially in the main tube body 10. The raw material enters the second inner tube body 50 from the raw material filling port 12, enters between the inner circumferential wall of the first inner tube body 40 and the outer circumferential wall of the second inner tube body 50 through the first flow gap 41, and enters between the outer circumferential wall of the first inner tube body 40 and the inner circumferential wall of the main tube body 10 through the second flow gap 51, and then enters the collection area 17 through the reaction through hole 21, and is discharged and collected from the collection port 11. By arranging the first inner tube body 40 and the second inner tube body 50 in the reaction zone 16, the second inner tube body 50 is inserted into the first inner tube body 40 to lengthen the path of the reactants in the main tube, so that the reaction is more complete.
[0036] Further, such as Figures 3 to 5 As shown, all the reaction holes 21 are arranged between the outer wall of the first inner tube body 40 and the inner wall of the main tube body 10 to ensure that all the reaction raw materials injected into the first inner tube body 40 by the second inner tube body 50 must pass through the second flow gap 51 before being discharged from the collection area 17, thereby preventing the reactants from directly entering the collection area 17 from the reaction holes 21 and being discharged.
[0037] Further, such as Figure 5 As shown, the inner tube body also includes a first connecting portion 52, one end of the first connecting portion 52 is connected to the outer wall of the second inner tube body 50, and the other end is connected to the inner wall of the first inner tube body 40, thereby improving the connection strength between the first inner tube body 40 and the second inner tube body 50, as well as the relative position stability between the first inner tube body 40 and the second inner tube body 50.
[0038] Further, such as Figure 5 As shown, the inner tube body further includes a second connecting portion 42, one end of which is connected to the outer wall of the first inner tube body 40, and the other end is connected to the inner wall of the main tube body 10. The connection strength between the first inner tube body 40 and the main tube body 10 and the relative position stability of the first inner tube body 40 and the main tube body 10 are improved.
[0039] Further, such as Figure 1 to Figure 2 As shown, the raw material filling port 12 includes a gas filling port 13 and a liquid filling port 14, and the liquid filling port 14 and the gas filling port 13 are respectively connected to one end of the second inner tube body 50 away from the first inner tube body 40. The raw material gas is filled through the gas filling port 13, and the raw material liquid is filled through the liquid filling port 14. The gas and liquid are filled simultaneously through separate filling ports, thereby improving the raw material operation efficiency and the production efficiency.
[0040] As one embodiment, as one embodiment, liquid phosphorus trichloride in the raw material is added from the liquid filling port 14 , and hydrogen in the raw material is added from the gas filling port 13 .
[0041] Further, such as Figure 5 As shown, the axial distance between the liquid filling port 14 and the baffle 20 is a, and the axial distance between the gas filling port 13 and the baffle 20 is b, where b>a. The gas filling port 13 is located at the rear side of the liquid filling port 14. When the raw material is filled, the gas is used to blow the liquid raw material into the reaction chamber 15, thereby improving the efficiency of the liquid raw material flowing into the reaction chamber 15.
[0042] Further, such as Figure 2 and Figure 4 As shown, the collecting port 11 is located below the filling port, the collecting port 11 is located outside the heating element 30, and the main body 10 is tilted as a whole. Since the collecting port 11 is located at a lower position, the product condenses into liquid at the collecting port 11, and the liquid product can flow out of the collecting port 11 smoothly for collection, avoiding blockage caused by solidification of the collecting port 11.
[0043] As one embodiment, Figure 2 and Figure 4 As shown, the heating element 30 surrounds and wraps around the outer circumference of the main body 10, and the collecting port 11 and the filling port of the main body 10 extend out of the heating element 30 respectively, so as to improve the heating uniformity of the main body 10. Further, the heating element 30 is a heating furnace.
[0044] In summary, the embodiment of the utility model provides a high-purity phosphorus hydrogenation reduction reaction tube, and the heating element 30 heats the main body 10 to make the raw material reach the reaction temperature. The reaction chamber 15 is divided into a reaction zone 16 and a collection zone 17 along the axial direction by the baffle 20. The reaction zone 16 is connected to the raw material filling port 12, and the raw materials phosphorus trichloride and hydrogen enter the reaction zone 16 through the raw material filling port 12, and react in the reaction zone 16. Under the action of the baffle 20, the reactant is blocked when it flows out in the direction of the collection zone 17, increasing the residence time of the reactant in the tube, and at the same time, the gas is more dispersed, so that the reaction is more complete, thereby increasing the output of phosphorus vapor, improving production efficiency, and reducing residual production raw materials, and improving production safety. After the phosphorus trichloride is gasified, it enters the collection zone 17 through the reaction through hole 21 and is discharged from the collection port 11, so as to realize the collection of the product phosphorus vapor.
[0045] The above are only preferred implementations of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and substitutions can be made without departing from the technical principles of the present invention. These improvements and substitutions should also be regarded as the protection scope of the present invention.
Claims
1. A high-purity phosphorus hydrogenation reduction reaction tube, characterized in that: The invention comprises a main body, a baffle and a heating element for heating the main body, wherein the main body is provided with a collecting port, a raw material filling port and a reaction chamber, the baffle is located in the reaction chamber and connected to the inner wall of the main body, the baffle is provided with a reaction through hole, the baffle divides the reaction chamber into a reaction zone and a collecting zone, the raw material filling port is connected to the reaction zone, the reaction zone is connected to the collecting zone through the reaction through hole, and the collecting zone is connected to the collecting port.
2. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 1, characterized in that: The reaction through hole is arranged on the upper part of the baffle.
3. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 1, characterized in that: The collecting port and the raw material filling port are respectively located at two ends of the main pipe body, and the baffle is located between the collecting port and the raw material filling port in the axial direction of the main pipe body.
4. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 3, characterized in that: It also includes an inner tube body, which includes a first inner tube body and a second inner tube body, one end of the first inner tube body is connected to the baffle, and the other end has a first flow gap with an end of the main tube body away from the collecting port, the second inner tube body is connected to the end of the main tube body away from the collecting port, one end of the second inner tube body extends into the first inner tube body and has a second flow gap with the baffle, and the other end extends out of the main tube body and is connected to the raw material filling port.
5. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 4, characterized in that: The reaction through holes are all arranged between the outer wall of the first inner tube body and the inner wall of the main tube body.
6. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 4, characterized in that: The inner tube body further includes a first connecting portion, one end of which is connected to the outer wall of the second inner tube body, and the other end of which is connected to the inner wall of the first inner tube body.
7. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 4, characterized in that: The inner tube body further includes a second connecting portion, one end of which is connected to the outer wall of the first inner tube body, and the other end of which is connected to the inner wall of the main tube body.
8. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 4, characterized in that: The raw material filling port includes a gas filling port and a liquid filling port, and the liquid filling port and the gas filling port are respectively connected to an end of the second inner tube body away from the first inner tube body.
9. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 8, characterized in that: The axial distance between the liquid filling port and the baffle is a, and the axial distance between the gas filling port and the baffle is b, where b>a.
10. The high-purity phosphorus hydrogenation reduction reaction tube according to claim 1, characterized in that: The collecting port is located below the filling port, the collecting port is located outside the heating element, and the main pipe is arranged in an inclined manner as a whole.