Reaction device for preparing NiP binary alloy through carbon thermal rapid reduction

Abstract

The invention discloses a reaction device for preparing NiP binary alloy through carbon thermal rapid reduction, and relates to the field of carbon thermal reduction devices.The reaction device comprises a reaction tank, a feeding pipeline is arranged in the reaction tank and distributed on the inner circle of the reaction tank by a circle in a spiral structure, the upper end of the feeding pipeline communicates with a feeding pipeline, and the lower end of the feeding pipeline communicates with a discharging pipeline; a feeding main pipe is arranged on the feeding pipeline and is used for being connected with a material pump for pumping a mixture into the reaction tank. The feeding pipeline is of a spiral structure, a mixture is preheated along the spiral channel before entering the reaction tank, the carbon thermal reaction efficiency is further improved, the mixing degree of the mixture can be improved, the silicon carbide rod heating plate is adopted, the temperature in the reaction tank can be rapidly increased to 800 DEG C, and the reaction time is remarkably shortened.

Description

Technical Field

[0001] This invention relates to the field of carbothermic reduction apparatus, and particularly to a reaction apparatus for the rapid carbothermic reduction of NiP binary alloys. Background Technology

[0002] Traditional methods for preparing NiP binary alloys mainly rely on techniques such as chemical deposition and electrochemical deposition, for example: Chemical vapor deposition (CVD) is used, but it requires high temperature and high pressure conditions. Typically, the reaction needs to be carried out at temperatures above 800°C and pressures of several atmospheres. This not only increases energy consumption but also places high demands on the equipment's high temperature and high pressure resistance. The main problems are low deposition rate and poor uniformity.

[0003] Electrochemical deposition requires high current densities, which increases energy consumption and may lead to electrode polarization, affecting deposition quality. A major problem is the poor stability of the electrolyte during deposition, as it contains various impurities that easily decompose and precipitate during the reaction, increasing production costs and operational complexity.

[0004] These methods share the following common problems: 1. Long reaction time: The reaction takes a long time to complete, resulting in low production efficiency; 2. Complex equipment: It requires complex equipment and processes, which increases production costs and operational difficulty.

[0005] Therefore, it is necessary to propose a carbothermic rapid reduction reaction device for preparing NiP binary alloys to solve the above problems. Summary of the Invention

[0006] The purpose of this invention is to provide a reaction apparatus for the rapid carbothermic reduction of NiP binary alloys, so as to solve the problems of low efficiency and high process difficulty in preparing NiP binary alloys by traditional technology.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a reaction apparatus for rapidly preparing NiP binary alloy by carbothermal reduction, comprising a reaction vessel, wherein a feed pipe is provided on the upper side of the reaction vessel, the feed pipe being used to feed a mixture of nickel oxide powder, ammonium dihydrogen phosphate and graphite powder, the mixture entering the reaction vessel after passing through the feed pipe, the mixture undergoing a carbothermal reduction reaction in the reaction vessel to generate NiP binary alloy and by-products; The reaction vessel is equipped with a feeding pipe inside. The feeding pipe is arranged in a spiral structure around the inner circle of the reaction vessel. The upper end of the feeding pipe is connected to the feed pipe. The feed pipe is equipped with a feed main pipe, which is used to connect to a material pump that pumps the mixture into the reaction vessel. The inner circle of the feeding pipe is equipped with a feed inlet, and a fourth solenoid valve is installed in the feed inlet.

[0008] Preferably, the reaction vessel is provided with a drive shaft inside, the drive shaft is vertically distributed, and the upper and lower ends of the drive shaft are respectively rotatably set at the upper and lower ends of the reaction vessel. A servo motor is fixedly installed on the upper surface of the reaction vessel by a motor bracket, and the lower end of the servo motor is fixedly connected to the upper end of the drive shaft. The drive shaft is provided with a smooth external thread section, and at least two smooth external thread sections are provided. A rotating wheel assembly is provided on the smooth external thread section. The rotating wheel assembly includes an outer ring, a blade and an inner ring. The inner ring of the inner ring has a smooth internal thread structure. The inner ring is connected to the smooth external thread section by a threaded engagement. Threaded limit rings are provided at both the upper and lower ends of the smooth external thread section. The outer ring is fitted over the inner ring, and the blades are fixedly connected between the inner ring of the outer ring and the outer ring of the inner ring. Multiple blades are provided, and the multiple blades are distributed at equal angles along the axis of the drive shaft.

[0009] Preferably, the bottom of the reaction vessel is provided with a discharge pipe and a support leg, and a first solenoid valve is provided on the discharge pipe.

[0010] Preferably, the upper end of the reaction vessel is also provided with an exhaust pipe, and the end of the exhaust pipe is provided with an exhaust treatment pipe; A support plate is fixedly welded to the inner wall of the lower end of the exhaust pipe. A vertical rod is fixedly installed on the upper surface of the support plate. A filter box is also installed in the exhaust pipe. A round hole is provided in the middle of the filter box. The vertical rod extends movably into the round hole. The two ends of the vertical rod are located above and below the filter box, respectively. Filter holes are provided on both the upper and lower surfaces of the filter box. An activated carbon filter layer is placed inside the filter box.

[0011] Preferably, an auxiliary cleaning pipe is also provided at the end of the exhaust pipe, and a fan is connected to the auxiliary cleaning pipe; Both the exhaust treatment pipe and the auxiliary cleaning pipe are equipped with a second solenoid valve.

[0012] Preferably, an electric heating plate is installed on the inner wall of the reaction vessel, and the electric heating plate is a silicon carbide heating plate.

[0013] Preferably, the reaction vessel is provided with a number of temperature measuring windows, which are distributed at equal intervals along the height of the reaction vessel.

[0014] Preferably, the feed pipe is provided with a feed auxiliary pipe, which is used to connect to a gas pump that pumps inert gas into the reaction vessel. Both the auxiliary feed pipe and the main feed pipe are equipped with a third solenoid valve.

[0015] Preferably, the feed inlet is connected to the inside of the feeding pipe, and multiple feed inlets are provided, which are distributed along the spiral trajectory of the feeding pipe.

[0016] Preferably, the upper end of the upright is connected to a limit nut by a threaded connection, and springs are fixedly provided on both the upper and lower surfaces of the filter box. The upper end of the spring on the upper surface of the filter box abuts against the lower surface of the limit nut, and the spring on the lower surface of the filter box abuts against the upper surface of the support plate.

[0017] The technical effects and advantages of this invention are as follows: 1. In this invention, the feeding pipe has a spiral structure. The mixture is preheated along the spiral channel before entering the reaction tank, which further improves the efficiency of the carbothermic reaction and can improve the mixing degree of the mixture. The silicon carbide heating plate can quickly raise the internal temperature of the reaction tank to 800°C, which significantly shortens the reaction time and the process is simple. 2. In this invention, a servo motor drives the drive shaft to rotate at high speed, which makes the mixture fully lifted and mixed in the reaction tank, increases the contact area between hot air and the mixture, ensures a more uniform reaction, and improves the purity of the product. 3. In this invention, inert gas is pumped into the reaction tank through the feed auxiliary pipe to remove air from the tank, prevent oxidation reaction, improve the safety of the reaction process, and can also drive the mixture to rise, making the carbothermic reduction reaction more efficient. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the reaction apparatus for the rapid carbothermic reduction of NiP binary alloys according to the present invention.

[0019] Figure 2 This is a schematic diagram of the reaction apparatus for the rapid carbothermic reduction of NiP binary alloys according to the present invention from another perspective.

[0020] Figure 3 This is a schematic diagram of the internal structure of the reaction apparatus for the rapid carbothermic reduction preparation of NiP binary alloys according to the present invention.

[0021] Figure 4 A cross-sectional view of the reaction apparatus for the carbothermic rapid reduction preparation of NiP binary alloys according to the present invention.

[0022] Figure 5 For the present invention Figure 4 Enlarged schematic diagram of the structure at point A in the middle.

[0023] Figure 6 This is a schematic diagram of the rotating wheel assembly structure of the present invention.

[0024] Figure 7 This is a schematic diagram of the feeding pipe structure of the present invention.

[0025] In the diagram: 1. Reaction vessel; 2. Servo motor; 3. Motor bracket; 4. Exhaust pipe; 5. Second solenoid valve; 6. Auxiliary cleaning pipe; 7. Exhaust treatment pipe; 8. Fan; 9. Feed pipe; 10. Auxiliary feed pipe; 11. Main feed pipe; 12. Temperature measuring window; 13. Discharge pipe; 14. Support leg; 15. Rotary wheel assembly; 16. Drive shaft; 17. Feeding pipe; 18. Electric heating plate; 19. Smooth external thread section; 20. Threaded limit ring; 21. Filter box; 22. Activated carbon filter layer; 23. Support plate; 24. Round hole; 25. Spring; 26. Upright pole; 27. Limit nut; 28. Feed inlet; 29. ​​Outer ring; 30. Blade; 31. Inner ring. Detailed Implementation

[0026] This invention provides a process for preparing NiP binary alloys by carbothermic rapid reduction, comprising: The first step involves a thermal reaction of nickel oxide powder, ammonium dihydrogen phosphate, and graphite powder. The reaction process includes: Carbothermic reduction and phosphating reactions; In the carbothermic reduction reaction, graphite powder reduces nickel oxide powder to metallic nickel powder, and the reaction temperature is usually above 800℃. During the phosphating reaction, ammonium dihydrogen phosphate decomposes at high temperature to produce phosphorus pentoxide and ammonia. Phosphorus pentoxide reacts with metallic nickel powder to produce nickel-phosphorus compound (NiP).

[0027] During the reaction, some side reactions may occur, such as the generation of carbon monoxide, which may further react with oxygen to generate carbon dioxide; the ammonia gas generated by the decomposition of ammonium dihydrogen phosphate may escape, and water vapor may be generated during the decomposition of ammonium dihydrogen phosphate.

[0028] The final product is mainly a nickel-phosphorus compound, and also contains some unreacted raw materials and byproducts, such as unreacted graphite powder, nickel oxide, and phosphorus pentoxide. The mixture after the reaction is further processed by washing, filtering, and drying to finally separate the nickel-phosphorus compound.

[0029] The present invention also provides, for example Figures 1-7The apparatus shown is a carbothermal rapid reduction reaction device for preparing NiP binary alloy, comprising: a reaction vessel 1, which is a cylindrical structure, with a feed pipe 9 on the upper side of the reaction vessel 1, through which a mixture of nickel oxide powder, ammonium dihydrogen phosphate and graphite powder is fed. The mixture enters the reaction vessel 1 after passing through the feed pipe 9, and undergoes a carbothermal reduction reaction in the reaction vessel 1 to generate nickel-phosphorus compound (NiP binary alloy) and by-products; a discharge pipe 13 is provided at the bottom of the reaction vessel 1, and a first solenoid valve is provided on the discharge pipe 13, which can discharge the material in the reaction vessel 1 when the first solenoid valve is opened.

[0030] refer to Figure 1 As shown, the upper end of the reaction tank 1 is also equipped with an exhaust pipe 4, and the end of the exhaust pipe 4 is equipped with an auxiliary cleaning pipe 6 and an exhaust treatment pipe 7. The auxiliary cleaning pipe 6 is connected to a fan 8, and the exhaust treatment pipe 7 is connected to an external waste gas treatment device. The waste gas generated in the reaction tank 1 can enter the interior of the waste gas treatment device for treatment through the exhaust treatment pipe 7, which is convenient and practical. When the NiP binary alloy production is stopped, the fan 8 can be started to supply water or airflow into the reaction tank 1 to achieve the purpose of cleaning the interior of the reaction tank 1. The exhaust treatment pipe 7 and the auxiliary cleaning pipe 6 are both equipped with a second solenoid valve 5 for convenient control.

[0031] refer to Figures 4 to 5 As shown, a support plate 23 is fixedly welded to the inner wall of the lower end of the exhaust pipe 4. A vertical rod 26 is fixedly installed on the upper surface of the support plate 23. A filter box 21 is also installed in the exhaust pipe 4. A round hole 24 is provided in the middle of the filter box 21. The vertical rod 26 extends movably into the round hole 24. The two ends of the vertical rod 26 are located above and below the filter box 21, respectively. The upper end of the vertical rod 26 is connected to a limit nut 27 by a threaded connection. Springs 25 are fixedly installed on both the upper and lower surfaces of the filter box 21. The upper end of the spring 25 on the upper surface of the filter box 21 abuts against the lower surface of the limit nut 27. The spring 25 on the lower surface of the filter box 21... The filter box 21 has filter holes on both the upper and lower surfaces, which are pressed against the upper surface of the support plate 23. An activated carbon filter layer 22 is placed inside the filter box 21. When the gas passes through the exhaust pipe 4, it can be initially filtered by the activated carbon filter layer 22 to prevent large particles from being discharged. Due to the instability of the airflow, the gas pushes the filter box 21 to compress or release the spring 25 in a reciprocating lifting motion, which causes large particles on the lower surface of the filter box 21 to detach and not adhere to and block the lower surface of the filter box 21. This ensures that the filter box 21 has a good filtration effect for a long time. After the equipment has been used for a certain period of time, regular maintenance is required.

[0032] refer to Figure 3As shown, an electric heating plate 18 is installed on the inner wall of the reaction vessel 1. The electric heating plate 18 uses a silicon carbide heating plate, which has a maximum operating temperature of 1500℃. When used below 800℃, it has a long service life and stable performance. The silicon carbide heating plate has high thermal efficiency and can quickly heat up to 800℃. It has good thermal shock resistance and high thermal stability, and can maintain good performance under frequent temperature changes. It has good chemical stability and is not easily oxidized or corroded, making it suitable for working in various atmospheres. When the mixture enters the reaction vessel 1, the electric heating plate 18 is activated, and the electric heating plate 18 heats the internal temperature of the reaction vessel 1 to about 800℃, so that the mixture undergoes a carbothermic reduction reaction.

[0033] refer to Figure 2 As shown, a number of temperature measuring windows 12 are provided on the reaction vessel 1. These temperature measuring windows 12 are distributed at equal intervals along the height of the reaction vessel 1. The internal temperature of the reaction vessel 1 can be measured by an infrared thermometer installed on the outside through the temperature measuring windows 12. This allows for the adjustment of the power or number of electric heating plates 18 according to actual needs, facilitating temperature control. The specific temperature control logic is the existing conventional operation and will not be described in detail here.

[0034] refer to Figure 4 and Figure 6 As shown, a drive shaft 16 is installed inside the reaction vessel 1. The drive shaft 16 is vertically distributed, and its upper and lower ends are rotatably mounted on the upper and lower ends of the reaction vessel 1, respectively. A servo motor 2 is fixedly mounted on the upper surface of the reaction vessel 1 via a motor bracket 3. The lower end of the servo motor 2 is fixedly connected to the upper end of the drive shaft 16. A smooth external thread section 19 is provided on the drive shaft 16. At least two smooth external thread sections 19 are provided. A rotating wheel assembly 15 is provided on the smooth external thread section 19. The rotating wheel assembly 15 includes an outer ring 2. 9. Blade 30 and inner ring 31. The inner ring 31 has a smooth internal thread structure. The inner ring 31 is connected to the smooth external thread section 19 by threaded engagement. Thread limit rings 20 are provided at both the upper and lower ends of the smooth external thread section 19. The thread limit rings 20 are used to limit the excessive vertical displacement of the inner ring 31. The outer ring 29 is sleeved on the outside of the inner ring 31. The blade 30 is fixedly connected between the inner ring of the outer ring 29 and the outer ring of the inner ring 31. Multiple blades 30 are provided. Multiple blades 30 are distributed at equal angles along the axis of the drive shaft 16.

[0035] When the servo motor 2 is started, the servo motor 2 drives the drive shaft 16 to rotate at high speed. After rotating for a certain period of time, it rotates in the opposite direction. Due to the rotational power of the drive shaft 16 combined with the centrifugal force of the rotating wheel assembly 15, the rotating wheel assembly 15 moves on the smooth external thread section 19. When the rotation direction of the servo motor 2 is switched, the rotating wheel assembly 15 can reciprocate up and down on the smooth external thread section 19, which can fully lift and mix the mixture inside the reaction tank 1. During the lifting process, the contact area between the hot air and the mixture is increased, so that the mixture can carry out the carbothermic reduction reaction more efficiently.

[0036] Servo motor 2 uses an ASDA-A2 series servo motor, which supports pulse control and analog control. It can achieve forward and reverse rotation through parameter settings and is suitable for use in the present invention and other fields of automation equipment.

[0037] refer to Figure 1 , Figure 3 , Figure 4 , Figure 6 and Figure 7 As shown, a feeding pipe 17 is provided inside the reaction tank 1. The feeding pipe 17 is arranged in a spiral structure around the inner circle of the reaction tank 1. The upper end of the feeding pipe 17 is connected to the feed pipe 9. The feed pipe 9 is provided with a feed auxiliary pipe 10 and a feed main pipe 11. Both the feed auxiliary pipe 10 and the feed main pipe 11 are provided with a third solenoid valve. The feed main pipe 11 is used to connect to a material pump that pumps the mixture into the reaction tank 1. The feed auxiliary pipe 10 is used to connect to a gas pump that pumps inert gas into the reaction tank 1. The inner circle of the feeding pipe 17 is provided with a feed port 28. A fourth solenoid valve is provided in the feed port 28. Multiple feed ports 28 are provided and distributed along the spiral trajectory of the feeding pipe 17.

[0038] When the material pump, the fourth solenoid valve, and the third solenoid valve on the feed main pipe 11 are started, the mixture enters the interior of the reaction tank 1 through the feed main pipe 11, the feed pipe 9, the feeding pipe 17, and the feed port 28 in sequence. The mixture enters the interior of the reaction tank 1 through multiple feed ports 28 in a sprayed state, which is relatively uniform and facilitates rapid carbothermic reduction reaction. In addition, the mixture entering the interior of the reaction tank 1 through multiple feed ports 28 will also impact the original mixture pile and lift it up, so that the mixture inside the reaction tank 1 is always in a chaotic state of being lifted up, which increases the heat exchange efficiency between the mixture and the hot air.

[0039] When the air pump, the fourth solenoid valve, and the third solenoid valve on the feed auxiliary pipe 10 are started, inert gas can be added to the reaction tank 1. The inert gas also enters the interior of the reaction tank 1 from multiple feed ports 28, which can also cause the mixture to be lifted.

[0040] The bottom of the reaction vessel 1 has support legs 14, and the entire equipment is installed on the ground.

[0041] It should be noted that, since the feed pipe 17 is located inside the reaction tank 1, the fourth solenoid valve at the feed inlet 28 needs to withstand a high temperature of 800℃. Therefore, the fourth solenoid valve is a high-temperature solenoid valve using heat transfer oil, which can withstand temperatures up to 800℃ or higher. Other types of solenoid valves can also be used, but will not be elaborated here. The first, second, and third solenoid valves operate in relatively good environments and use conventional models such as ASCO solenoid valves. The material pumps selected are: QBF-65 pneumatic diaphragm pump, XLQ-P stainless steel powder pneumatic diaphragm pump, or JT.G series low-pressure continuous transfer pump. The air pump used is a Teride 4-inch Power Star 4B air-driven air pump for conveying inert gas: nitrogen.

[0042] In summary, the feeding pipe 17 in this invention not only improves the mixing degree of the mixture, but also allows the mixture to be preheated along the spiral channel before entering the reaction tank 1, thereby improving the efficiency of the carbothermic reaction.

Claims

1. A reaction device for preparing NiP binary alloy by carbon thermal rapid reduction, comprising a reaction tank (1), characterized in that: The upper side of the reaction vessel (1) is provided with a feed pipe (9), which allows a mixture of nickel oxide powder, ammonium dihydrogen phosphate and graphite powder to enter. The mixture enters the reaction vessel (1) after passing through the feed pipe (9), and the mixture undergoes a carbothermic reduction reaction in the reaction vessel (1) to generate NiP binary alloy and by-products. The reaction vessel (1) is provided with a feeding pipe (17) inside. The feeding pipe (17) is distributed in a spiral structure around the inner circle of the reaction vessel (1). The upper end of the feeding pipe (17) is connected to the feed pipe (9). The feed pipe (9) is provided with a feed main pipe (11). The feed main pipe (11) is used to connect to a material pump that pumps the mixture into the reaction vessel (1). The inner circle of the feeding pipe (17) is provided with a feed inlet (28). A fourth solenoid valve is provided in the feed inlet (28). 2.The reaction device for preparing NiP binary alloy by carbon thermal rapid reduction according to claim 1, characterized in that: The reaction vessel (1) is equipped with a drive shaft (16) inside. The drive shaft (16) is vertically distributed. The upper and lower ends of the drive shaft (16) are respectively rotatably set at the upper and lower ends of the reaction vessel (1). A servo motor (2) is fixedly installed on the upper surface of the reaction vessel (1) through a motor bracket (3). The rotating shaft at the lower end of the servo motor (2) is fixedly connected to the upper end of the drive shaft (16). The drive shaft (16) is provided with a smooth external thread section (19), and there are at least two smooth external thread sections (19). A rotating wheel assembly (15) is provided on the smooth external thread section (19). The rotating wheel assembly (15) includes an outer ring (29), a blade (30) and an inner ring (31). The inner ring (31) has a smooth internal thread structure. The inner ring (31) is connected to the smooth external thread section (19) by a threaded fit. Threaded limit rings (20) are provided at both the upper and lower ends of the smooth external thread section (19). The outer ring (29) is sleeved on the outside of the inner ring (31), and the blades (30) are fixedly connected between the inner ring of the outer ring (29) and the outer ring of the inner ring (31). Multiple blades (30) are provided, and the multiple blades (30) are distributed at equal angles along the axis of the drive shaft (16). 3.The reaction device for preparing NiP binary alloy by carbon thermal rapid reduction according to claim 1, characterized in that: The bottom of the reaction vessel (1) is provided with a discharge pipe (13) and a support leg (14), and a first solenoid valve is provided on the discharge pipe (13). 4.The reaction device for preparing NiP binary alloy by carbon thermal rapid reduction according to claim 1, characterized in that: The upper end of the reaction vessel (1) is also provided with an exhaust pipe (4), and the end of the exhaust pipe (4) is provided with an exhaust treatment pipe (7). A support plate (23) is fixedly welded to the inner wall of the lower end of the exhaust pipe (4). A vertical rod (26) is fixedly installed on the upper surface of the support plate (23). A filter box (21) is also installed in the exhaust pipe (4). A round hole (24) is provided in the middle of the filter box (21). The vertical rod (26) extends into the round hole (24). The two ends of the vertical rod (26) are located above and below the filter box (21) respectively. Filter holes are provided on both the upper and lower surfaces of the filter box (21). An activated carbon filter layer (22) is placed inside the filter box (21).

5. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 4, characterized in that: An auxiliary cleaning pipe (6) is also provided at the end of the exhaust pipe (4), and a fan (8) is connected to the auxiliary cleaning pipe (6). A second solenoid valve (5) is installed on both the exhaust treatment pipe (7) and the auxiliary cleaning pipe (6).

6. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 1, characterized in that: An electric heating plate (18) is installed on the inner wall of the reaction vessel (1), and the electric heating plate (18) uses a silicon carbide heating plate.

7. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 1, characterized in that: The reaction vessel (1) is provided with a temperature measuring window (12), and there are several temperature measuring windows (12) distributed at equal distances along the height direction of the reaction vessel (1).

8. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 1, characterized in that: The feed pipe (9) is provided with a feed auxiliary pipe (10), which is used to connect to a gas pump that pumps inert gas into the reaction tank (1). Both the feed auxiliary pipe (10) and the feed main pipe (11) are equipped with a third solenoid valve.

9. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 1, characterized in that: The feed inlet (28) is connected to the inside of the feeding pipe (17), and there are multiple feed inlets (28), which are distributed along the spiral trajectory of the feeding pipe (17).

10. The reaction apparatus for rapid carbothermic reduction of NiP binary alloys according to claim 4, characterized in that: The upper end of the upright (26) is connected to the limit nut (27) by threaded connection. Springs (25) are fixedly installed on the upper and lower surfaces of the filter box (21). The upper end of the spring (25) on the upper surface of the filter box (21) abuts against the lower surface of the limit nut (27), and the spring (25) on the lower surface of the filter box (21) abuts against the upper surface of the support plate (23).

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