Preparation process and device of nickel-phosphorus intermediate alloy

Abstract

The present application relates to the field of alloy material preparation, and particularly relates to a preparation process and device of nickel-phosphorus intermediate alloy. The preparation device of the nickel-phosphorus intermediate alloy comprises a medium-frequency furnace, a crucible assembly, a pressing cover mechanism, a nickel liquid injection mechanism, a nickel liquid containing and conveying mechanism, a gas charging and discharging system, a lifting device and a fixing frame. The medium-frequency furnace comprises a furnace body, a furnace cover and a base, and the furnace body and the base are in a split structure. The crucible assembly comprises a crucible and a two-stage throttle orifice plate assembly, and the two-stage throttle orifice plate assembly comprises an upper orifice plate, a lower orifice plate and a spacer block. The key points of the process for preparing the nickel-phosphorus intermediate alloy by using the device are as follows: nickel and phosphorus are put into the crucible in the medium-frequency furnace, the medium-frequency furnace is filled with nitrogen, the nickel and the phosphorus are heated and mixed and melted in the nitrogen atmosphere, and then the nickel-phosphorus intermediate alloy product is obtained after casting and cooling. The present application has the characteristics of simple process, low energy consumption, high production efficiency, easy quality control, environmental protection requirement, and low preparation cost.

Description

Technical Field

[0001] This invention relates to the field of alloy material preparation, and in particular to a process for preparing a nickel-phosphorus master alloy. This invention also relates to an apparatus for preparing a nickel-phosphorus master alloy. Background Technology

[0002] Nickel-based brazing filler metals are mainly used for welding stainless steel. Phosphorus needs to be added during the smelting of nickel-based brazing filler metals. In order to better control the phosphorus content in nickel-based brazing filler metals, the addition of phosphorus is mainly accomplished in the form of nickel-phosphorus alloys.

[0003] Red phosphorus has a boiling point of 350℃, sublimates when heated to 416℃, has an ignition point of 260℃, and a density of 2.34 g / cm³. 3 The melting point of nickel ingots is 1453℃, and their density is 8.902 g / cm³. 3 If conventional smelting processes are used, red phosphorus will sublimate or burn before the nickel ingot melts during heating; even when molten nickel is poured onto red phosphorus, its low density causes it to float to the surface and burn or sublimate. Therefore, it is necessary to find a method that allows sufficient contact time between red phosphorus and molten nickel, ensuring thorough mixing and melting, reducing sublimation and combustion of red phosphorus, and obtaining a nickel-phosphorus alloy with a high phosphorus content, while simultaneously protecting the environment. However, existing nickel-phosphorus alloy preparation processes suffer from drawbacks such as high difficulty in quality control, significant environmental pollution, large emissions of harmful substances during preparation, complex operation, and high production costs. Summary of the Invention

[0004] To address the shortcomings of existing nickel-phosphorus alloy preparation processes, such as high difficulty in quality control, significant environmental pollution, large emissions of harmful substances during preparation, complex operation, and high cost, the present invention aims to provide a simple, efficient, easy-to-control, environmentally friendly, and low-cost preparation process for nickel-phosphorus master alloys. Furthermore, the present invention aims to provide an apparatus for preparing nickel-phosphorus master alloys.

[0005] The technical solution adopted for the purpose of this invention is achieved through the following method: a preparation process for a nickel-phosphorus master alloy, the key points of which are: placing nickel and phosphorus into a crucible in the furnace cavity of an intermediate frequency furnace, filling the furnace cavity with nitrogen gas, and then heating, mixing, and melting the nickel and phosphorus in the nitrogen atmosphere through the intermediate frequency furnace, followed by casting and cooling to obtain the nickel-phosphorus master alloy product; wherein, the nickel used in the preparation of the nickel-phosphorus master alloy is electrolytic nickel, and the phosphorus used is red phosphorus;

[0006] Furthermore, in the preparation process of the nickel-phosphorus master alloy, the ratio between red phosphorus and electrolytic nickel is determined by mass percentage, wherein the mass percentage of red phosphorus is 0.5-20.0% and the mass percentage of electrolytic nickel is 80.0-99.5%.

[0007] Furthermore, the preparation process of the nickel-phosphorus master alloy is realized through a nickel-phosphorus master alloy preparation apparatus. This apparatus includes a medium-frequency furnace, a crucible assembly, a capping mechanism, a nickel liquid injection mechanism, a nickel liquid holding and conveying mechanism, a gas filling and discharging system, a lifting device, and a fixing frame. The medium-frequency furnace includes a furnace body, a furnace cover, and a base. The furnace body and the base are separate structures. The furnace body is fixed to the fixing frame. A sealing ring is provided between the base and the furnace body. An upper heating coil and a lower heating coil are arranged on the inner wall of the furnace body in a top-to-bottom order. A heat insulation pad is provided on the top surface of the base. The base is located on top of the lifting device, which is placed on the ground. The crucible assembly includes a crucible and a double-stage... A throttling orifice plate assembly, wherein the dual-stage throttling orifice plate assembly includes an upper orifice plate, a lower orifice plate, and three or more spacers, the spacers being evenly distributed between the upper and lower orifice plates, and the dual-stage throttling orifice plate assembly cooperating with the crucible; a pressure cap mechanism is disposed above the crucible assembly for pressing down the upper orifice plate of the dual-stage throttling orifice plate assembly; a nickel liquid injection mechanism is disposed above the intermediate frequency furnace for injecting nickel liquid into the crucible; a nickel liquid holding and conveying mechanism is disposed on one side of the nickel liquid injection mechanism for holding and conveying nickel liquid to the nickel liquid injection mechanism; a gas charging and discharging system includes a charging pipe and a discharging pipe, the outlet of the charging pipe and the inlet of the discharging pipe being disposed above the inner cavity of the furnace body. In use, after the red phosphorus is placed into the crucible, the crucible is placed on the heat insulation pad on the top surface of the base, and the dual-stage throttling orifice plate assembly is placed on the red phosphorus inside the crucible. At this time, the lower orifice plate in the dual-stage throttling orifice plate assembly covers the red phosphorus inside the crucible.

[0008] Furthermore, the heat insulation pad is made of high-temperature cement material, and the base is made of stainless steel material;

[0009] Furthermore, the crucible is made of graphite clay material;

[0010] Furthermore, the spacer block is made of graphite clay material, and the spacer block is cylindrical with a diameter of 10-50 mm and a height of 30-80 mm;

[0011] Furthermore, the upper perforated plate is made of graphite clay material, with an edge thickness of 13-35 mm and a middle thickness of 10-30 mm. The edge of the upper perforated plate can fit against the inner wall of the crucible. The top surface of the upper perforated plate is an arc surface, and the bottom surface of the upper perforated plate is a flat surface. The purpose of this design is to allow the molten nickel to flow downward from the through hole in the middle of the upper perforated plate when it is poured into the crucible.

[0012] Furthermore, the upper perforated plate has one or more through holes, the diameter of which is 3 to 15 mm;

[0013] Furthermore, the through hole one on the upper perforated plate consists of one vertical hole one and one to three oblique holes one, with the vertical hole one on top and the oblique holes one on the bottom, wherein the angle between the axis of the oblique hole one and the axis of the vertical hole one is 30° to 60°; the through hole one on the upper perforated plate adopts this design to reduce the resistance when the nickel liquid flows downward, making it difficult for the red phosphorus in the crucible to float upward, thereby reducing the sublimation and combustion loss of red phosphorus;

[0014] Furthermore, the lower perforated plate is made of graphite clay material, and the thickness of the lower perforated plate is 10-30mm;

[0015] Furthermore, the lower perforated plate has one or more through holes II, the diameter of which is 3-15mm;

[0016] Furthermore, the second through hole on the lower perforated plate consists of one vertical hole and one to three oblique holes, with the vertical hole at the top and the oblique holes at the bottom. The angle between the axis of the oblique hole and the axis of the vertical hole is 30° to 60°. This design of the second through hole on the lower perforated plate reduces the resistance when the molten nickel flows from top to bottom into the crucible, making it difficult for the red phosphorus in the crucible to float. This allows the red phosphorus and molten nickel to mix and melt fully during the smelting of the nickel-phosphorus intermediate alloy, reducing the sublimation and combustion loss of red phosphorus.

[0017] Furthermore, the vertical hole two on the second through hole of the lower perforated plate is located 30-50mm from the edge of the lower perforated plate and more than 80mm from the center of the lower perforated plate; the vertical hole one on the first through hole of the upper perforated plate is located 20-50mm from the center of the upper perforated plate. The vertical hole one on the first through hole of the upper perforated plate and the vertical hole two on the second through hole of the lower perforated plate are not on the same axis. In the process of smelting nickel-phosphorus intermediate alloy, if the red phosphorus in the crucible floats from the lower perforated plate, it will not directly enter the first through hole of the upper perforated plate but will float directly to the surface of the nickel liquid and sublimate or burn. The upper and lower perforated plates are separated by a spacer block, the openings are not on the same axis, and the through hole structure adopts a design with the upper section vertical and the lower end inclined, which lengthens the upward floating path of the red phosphorus during the smelting process, increases the resistance, and thus makes it more likely to be fully mixed and melted with the nickel liquid and not sublimate and overflow, resulting in loss.

[0018] Furthermore, the pressure cap mechanism includes a pressure cap plate, a pressure rod, and a lifting mechanism. The lower end of the pressure rod is connected to the pressure cap plate, and the upper end of the pressure rod is connected to the lifting mechanism. The bottom of the pressure cap plate is provided with a foot, and the pressure cap plate is connected to the upper orifice plate of the dual-stage throttling orifice plate assembly through the foot. Its function is to prevent the pressure cap plate from blocking the through hole 1 on the upper orifice plate, ensuring that the through hole 1 on the upper orifice plate is unobstructed. The lifting mechanism is located above the furnace cover of the medium-frequency furnace. The lifting mechanism presses down on the upper orifice plate through the pressure rod and the pressure cap plate. Its function is to prevent the upper orifice plate and the lower orifice plate from floating up during smelting after the nickel liquid is poured into the crucible, stably pressing down the red phosphorus and preventing the red phosphorus from overflowing from the edge of the crucible.

[0019] Furthermore, the pressure rod and the pressure plate are made of graphite clay material.

[0020] Furthermore, the nickel liquid injection mechanism is a funnel made of graphite clay material.

[0021] Furthermore, the gas charging and discharging system includes a charging pipe and an exhaust pipe. The outlet of the charging pipe is located above the inner cavity of the furnace body, and the inlet of the charging pipe is connected to a nitrogen source. The nitrogen source can be a nitrogen cylinder, nitrogen tank, or nitrogen generator. A charging valve is provided on the charging pipe. The inlet of the exhaust pipe is located above the inner cavity of the furnace body, and the outlet of the exhaust pipe is connected to a smoke removal device.

[0022] Furthermore, the nickel liquid holding and conveying mechanism is a ladle, which is made of graphite clay material.

[0023] Furthermore, a process for preparing nickel-phosphorus master alloys using an apparatus for preparing nickel-phosphorus master alloys includes the following steps:

[0024] (1) Weigh red phosphorus and electrolytic nickel according to the proportions;

[0025] (2) Melt the weighed nickel blocks into liquid nickel and place them in a ladle for later use;

[0026] (3) Place the weighed red phosphorus into the crucible and level it;

[0027] (4) Cover the red phosphorus in the crucible with the lower perforated plate;

[0028] (5) Place several spacer blocks evenly along the top edge of the lower perforated plate, and place the upper perforated plate on the spacer blocks;

[0029] (6) Turn on the lowering switch of the lifting device. After the base descends to the lower stop position, place the crucible on the heat insulation pad on the base. Then turn on the raising switch of the lifting device. The base moves upward and sends the crucible into the cavity of the medium frequency furnace body. The upper hole plate is pressed by the pressure rod and pressure plate cover in the lifting mechanism located above the furnace cover of the medium frequency furnace.

[0030] (7) Open the gas filling valve on the gas filling pipe and inject high-purity nitrogen into the furnace cavity of the medium frequency furnace. Then turn on the power switch of the upper heating coil to heat it.

[0031] (8) After the temperature inside the furnace cavity of the medium frequency furnace rises to the set temperature, turn off the power switch of the upper heating coil to stop heating, and then pour the molten nickel in the ladle into the crucible inside the furnace cavity of the medium frequency furnace through the funnel. At the same time, the molten nickel entering the crucible flows into the red phosphorus through the through hole one on the upper plate and the through hole two on the lower plate and is mixed and melted.

[0032] (9) After the molten nickel in the ladle is poured into the crucible inside the furnace cavity of the medium frequency furnace through the funnel, the power switches of the upper heating coil and the lower heating coil are turned on to start heating. At this time, the medium frequency furnace is in the state of smelting nickel-phosphorus intermediate alloy. During the smelting of nickel-phosphorus intermediate alloy, due to the low density of red phosphorus and the high density of molten nickel, red phosphorus will overflow upward through the through hole 2 of the lower orifice plate and the through hole 1 of the upper orifice plate, while molten nickel will enter the bottom of the crucible through the through hole 1 of the upper orifice plate and the through hole 2 of the lower orifice plate, so that red phosphorus and molten nickel gradually mix and melt. Turning on the power switches of the upper heating coil and the lower heating coil will stir the molten nickel in the crucible, so that red phosphorus will gradually mix and melt into the molten nickel. If flue gas is generated during the smelting of nickel-phosphorus intermediate alloy, the flue gas will be discharged to the smoke removal equipment for treatment through the exhaust pipe.

[0033] (10) After the red phosphorus and nickel liquid are fully mixed and melted, the pressure rod and pressure plate cover are moved up by the lifting mechanism. The upper orifice plate, lower orifice plate and spacer block will float to the surface of the melt. Continue smelting for 3 to 10 minutes to make the melt composition uniform.

[0034] (11) Turn off the power switches of the upper heating coil and the lower heating coil, close the gas filling valve, turn on the lowering switch of the lifting device, and after the base is lowered to the lower stop position, move the crucible out of the furnace cavity of the medium frequency furnace. Transfer the crucible to the casting mold edge through the crucible transfer device, use special tools to clamp out the upper hole plate, lower hole plate and spacer block, and finally cast the nickel-phosphorus intermediate alloy melt in the crucible to obtain the nickel-phosphorus alloy product.

[0035] In the above-mentioned process step (7) of preparing nickel-phosphorus master alloy using a nickel-phosphorus master alloy preparation device, the flow rate of the injected high-purity nitrogen gas is 1.0 L / min or more, and the nitrogen charging time is 0.1 min or more; the purpose of charging nitrogen gas is to prevent a small amount of red phosphorus from escaping during the smelting of nickel-phosphorus master alloy, so that the red phosphorus will not burn and generate phosphorus pentoxide to escape from the medium frequency furnace.

[0036] In the above-mentioned process step (7) of preparing nickel-phosphorus master alloy using a nickel-phosphorus master alloy preparation device, the crucible preheating time is 1 min or more.

[0037] In step (8) of the above-mentioned process for preparing nickel-phosphorus master alloy using a nickel-phosphorus master alloy preparation device, the temperature of the nickel liquid is 1600℃~1800℃.

[0038] In step (9) of the above-mentioned process for preparing nickel-phosphorus master alloy using a nickel-phosphorus master alloy preparation device, the upper and lower heating coils are turned on to electromagnetically stir the molten nickel in the crucible. Red phosphorus slowly floats to the surface while the molten nickel gradually flows down through the upper and lower orifice plates. The red phosphorus gradually dissolves into the molten nickel during stirring. Due to the unique structure of the dual-stage throttling orifice plate assembly, the red phosphorus floats relatively slowly and mixes into the molten nickel before reaching the surface, reducing the risk of red phosphorus floating to the surface and escaping from the induction furnace, thus preventing environmental pollution. This allows the red phosphorus to gradually mix into the molten nickel.

[0039] In the above-mentioned process step (10) of preparing nickel-phosphorus master alloy using a nickel-phosphorus master alloy preparation device, the reason for moving the pressure rod and pressure plate cover upward by the lifting mechanism and continuing smelting for 3 to 10 minutes is that the content of the melt in the bottom of the crucible, the area between the upper and lower perforated plates and the area above the upper perforated plate is different. It is necessary to remove the upper and lower perforated plates and continue smelting for a certain period of time in order to make the content in the crucible uniform.

[0040] In the aforementioned apparatus for preparing nickel-phosphorus master alloys, the upper heating coil is located on the upper inner wall of the furnace cavity of the intermediate frequency furnace. Its main function is to preheat the upper part of the crucible, the funnel, the upper perforated plate, the lower perforated plate, the spacer block, the pressure plate, and the pressure rod, removing moisture from these components to prevent splashing of molten nickel during pouring. These components reach a certain temperature to prevent the molten nickel from freezing after pouring. Because the upper heating coil is located on the upper inner wall of the furnace cavity of the intermediate frequency furnace, it does not heat the bottom of the crucible, thus maintaining the temperature of red phosphorus on the lower perforated plate below 300°C, preventing red phosphorus sublimation at this location.

[0041] The preparation process of the nickel-phosphorus master alloy of the present invention has the following characteristics compared with the existing nickel-phosphorus alloy preparation processes:

[0042] During the smelting process, the sealing effect of the two-stage throttling orifice plate assembly and the use of a nitrogen atmosphere in the furnace isolate the air, reduce phosphorus volatilization, and significantly reduce burn-off and environmental pollution.

[0043] The process is simple, energy-efficient, and low-cost;

[0044] It has high production efficiency and is easy to control quality. Attached Figure Description

[0045] Figure 1 This is a schematic diagram of the apparatus for preparing a nickel-phosphorus master alloy according to the present invention.

[0046] Figure 2 This is a schematic diagram of the structure of a two-stage throttling orifice plate assembly.

[0047] In the appendix Figure 1 and attached Figure 2 In the diagram, 1 represents an intermediate frequency furnace; 1a represents the furnace body; 1b represents the furnace cover; 1c represents the upper heating coil; 1d represents the lower heating coil; 1e represents the base; 1f represents the sealing ring; 1g represents the heat insulation pad; 2 represents the crucible assembly; 2a represents the crucible; 2b represents the upper perforated plate; 2b1 represents through hole one; 2b11 represents vertical hole one; 2b12 represents oblique hole one; 2c represents the lower perforated plate; 2c1 represents through hole two; 2c11 represents vertical hole two; 2c12 represents oblique hole two; 2d represents the spacer block; 3 represents the pressure cap mechanism; 3a represents the pressure cap plate; 3a1 represents the base; 3b represents the pressure rod; 3c represents the lifting mechanism; 4 represents the funnel; 5 represents the ladle; 6 represents the gas filling pipe; 6a represents the gas filling valve; 7 represents the exhaust pipe; 8 represents the lifting device; 9 represents red phosphorus; 10 represents molten nickel; 11 represents the fixing frame; and 12 represents the ground. Detailed Implementation

[0048] The present invention will be further described in detail below with reference to the embodiments shown in the accompanying drawings:

[0049] Example 1

[0050] See attached document Figure 1 and attached Figure 2 A process for preparing a nickel-phosphorus master alloy containing 16% phosphorus, the process comprising the following steps:

[0051] (1) Weigh out 83.5 kg of electrolytic nickel and 16.5 kg of red phosphorus;

[0052] (2) The weighed nickel blocks are smelted and melted into nickel liquid 10 and placed in ladle 5 for later use;

[0053] (3) Place red phosphorus 9 into crucible 2a with a capacity of 150 kg and level it;

[0054] (4) Cover the red phosphorus 9 inside crucible 2a with a perforated plate 2c;

[0055] (5) Place six spacer blocks 2d evenly along the top edge of the lower perforated plate 2c, and place the upper perforated plate 2b on the spacer blocks 2d;

[0056] (6) Turn on the lowering switch of the lifting device 8. After the base 1e is lowered to the lower stop position, place the crucible 2a on the heat insulation pad 1g on the base 1e. Then turn on the raising switch of the lifting device 8 and send the crucible 2a into the furnace body 1a cavity of the medium frequency furnace 1. Press the upper hole plate 2b tightly through the pressure rod 3b and pressure plate cover 3a in the lifting mechanism 3c.

[0057] (7) Open the gas filling valve 6a on the gas filling pipe 6 and inject high-purity nitrogen into the furnace body 1a cavity of the medium frequency furnace 1 at a flow rate of 3L / min. Then turn on the power switch of the upper heating coil 1c to heat it.

[0058] (8) After heating for 5 minutes, turn off the power switch of the upper heating coil 1c to stop heating, and then pour the nickel liquid 10 in the ladle 5 into the crucible 2a in the furnace body 1a cavity of the medium frequency furnace 1 through the funnel 4;

[0059] (9) After the molten nickel 10 in the ladle 5 is completely poured into the crucible 2a in the furnace body 1a cavity of the medium frequency furnace 1 through the funnel 4, the power switches of the upper heating coil 1c and the lower heating coil 1d are turned on at the same time to start smelting for 20 minutes.

[0060] (10) After the red phosphorus 9 and nickel liquid 10 are fully mixed and melted, the pressure rod 3b and pressure plate cover 3a are moved up by the lifting mechanism 3c, and the smelting continues for 5 minutes to make the melt composition uniform.

[0061] (11) Turn off the power switches of the upper heating coil 1c and the lower heating coil 1d, turn off the gas valve 6a, turn on the lowering switch of the lifting device 8, and after the base 1e descends to the lower stop position, move the crucible 2a out of the furnace body 1a cavity of the medium frequency furnace 1. Transfer the crucible 2a to the casting mold edge through the crucible transfer device, use special tools to clamp out the upper hole plate 2b, the lower hole plate 2c and the spacer block 2d, and finally cast the nickel-phosphorus intermediate alloy melt in the crucible 2a to obtain the nickel-phosphorus alloy product.

[0062] (12) According to the analysis, the phosphorus content of the nickel-phosphorus alloy product is 15.88%.

[0063] In step (4) above, the thickness of the lower perforated plate 2c is 25mm. Six through holes 2c1 with a diameter of 10mm are evenly distributed on the lower perforated plate 2c at a position 30mm away from the edge. The through holes 2c1 consist of one vertical hole 2c11 and two oblique holes 2c12. The vertical hole 2c11 is on top and the oblique holes 2c12 are on the bottom. The angle between the axis of the oblique hole 2c12 and the axis of the vertical hole 2c11 is 45°.

[0064] In step (5) above, the spacer block 2d is cylindrical with a diameter of 40 mm and a height of 50 mm.

[0065] In step (5) above, the top surface of the upper perforated plate 2b is an arc surface, the bottom surface of the upper perforated plate 2b is a plane, the edge thickness of the upper perforated plate 2b is 35mm, the middle thickness is 25mm, and six through holes 2b1 with a diameter of 10mm are evenly distributed on the upper perforated plate 2b at a position 30mm away from the center. The through hole 2b1 consists of a vertical hole 2b11 and two oblique holes 2b12. The vertical hole 2b11 is on top, the oblique hole 2b12 is on the bottom, and the angle between the axis of the oblique hole 2b12 and the axis of the vertical hole 2b11 is 45°.

[0066] Example 2

[0067] See attached document Figure 1 and attached Figure 2 A process for preparing a nickel-phosphorus master alloy containing 10% phosphorus, the process comprising the following steps:

[0068] (1) Weigh out 89.5 kg of electrolytic nickel and 10.5 kg of red phosphorus;

[0069] (2) The weighed nickel blocks are smelted and melted into nickel liquid 10 and placed in ladle 5 for later use;

[0070] (3) Place red phosphorus 9 into crucible 2a with a capacity of 150 kg and level it;

[0071] (4) Cover the red phosphorus 9 inside crucible 2a with a perforated plate 2c;

[0072] (5) Place six spacer blocks 2d evenly along the top edge of the lower perforated plate 2c, and place the upper perforated plate 2b on the spacer blocks 2d;

[0073] (6) Turn on the lowering switch of the lifting device 8. After the base 1e is lowered to the lower stop position, place the crucible 2a on the heat insulation pad 1g on the base 1e. Then turn on the raising switch of the lifting device 8 and send the crucible 2a into the cavity of the furnace body 1a of the medium frequency furnace 1. Press the upper hole plate 2b through the pressure rod 3b and the pressure plate cover 3a in the lifting mechanism 3c.

[0074] (7) Open the gas filling valve 6a on the gas filling pipe 6 and inject high-purity nitrogen into the cavity of the furnace body 1a of the medium frequency furnace 1 at a flow rate of 3L / min. Then turn on the power switch of the upper heating coil 1c to heat it.

[0075] (8) After heating for 5 minutes, turn off the power switch of the upper heating coil 1c to stop heating, and then pour the nickel liquid 10 in the ladle 5 into the crucible 2a in the furnace body 1a cavity of the medium frequency furnace 1 through the funnel 4;

[0076] (9) After the molten nickel 10 in the ladle 5 is completely poured into the crucible 2a in the furnace body 1a cavity of the medium frequency furnace 1 through the funnel 4, the power switches of the upper heating coil 1c and the lower heating coil 1d are turned on at the same time to start smelting for 20 minutes.

[0077] (10) After the red phosphorus 9 and nickel liquid 10 are fully mixed and melted, the pressure rod 3b and pressure plate cover 3a are moved up by the lifting mechanism 3c, and the smelting continues for 5 minutes to make the melt composition uniform.

[0078] (11) Turn off the power switches of the upper heating coil 1c and the lower heating coil 1d, turn off the gas valve 6a, turn on the lowering switch of the lifting device 8, and after the base 1e descends to the lower stop position, move the crucible 2a out of the furnace body 1a cavity of the medium frequency furnace 1. Transfer the crucible 2a to the casting mold edge through the crucible transfer device, use special tools to clamp out the upper hole plate 2b, the lower hole plate 2c and the spacer block 2d, and finally cast the nickel-phosphorus intermediate alloy melt in the crucible 2a to obtain the nickel-phosphorus alloy product.

[0079] (12) According to the analysis, the phosphorus content of the nickel-phosphorus alloy is 10.01%.

[0080] In step (4) above, the structure of the lower perforated plate 2c is the same as that of the lower perforated plate 2c in Example 1.

[0081] In step (5) above, the structure of the spacer block 2d is the same as that of the spacer block 2d in Example 1.

[0082] In step (5) above, the structure of the upper perforated plate 2b is the same as that of the upper perforated plate 2b in embodiment 1.

[0083] Example 3

[0084] See attached document Figure 1 and attached Figure 2 An apparatus for preparing a nickel-phosphorus master alloy is disclosed. The apparatus includes a medium-frequency furnace 1, a crucible assembly 2, a capping mechanism 3, a nickel liquid injection mechanism, a nickel liquid holding and conveying mechanism, a gas filling and discharging system, a lifting device 8, and a fixing frame 11. The medium-frequency furnace 1 includes a furnace body 1a, a furnace cover 1b, and a base 1e. The furnace body 1a and the base 1e are separate structures. The furnace body 1a is fixed to the fixing frame 11. A sealing ring 1f is provided between the base 1e and the furnace body 1a. An upper heating coil 1c and a lower heating coil 1d are arranged on the inner wall of the furnace body 1a in a top-to-bottom order. A heat insulation pad 1g is provided on the top surface of the base 1e. The base 1e is located on top of the lifting device 8, which is placed on the ground 12. The crucible assembly 2 includes a crucible 2a and a two-stage section... A flow orifice plate assembly, wherein the dual-stage throttling orifice plate assembly includes an upper orifice plate 2b, a lower orifice plate 2c, and three or more spacer blocks 2d, the spacer blocks 2d being evenly distributed between the upper orifice plate 2b and the lower orifice plate 2c; the dual-stage throttling orifice plate assembly cooperates with the crucible 2a; a pressure cap mechanism 3 is disposed above the crucible assembly 2, used to press down the upper orifice plate 2b of the dual-stage throttling orifice plate assembly; a nickel liquid injection mechanism is disposed above the intermediate frequency furnace 1, used to inject nickel liquid into the crucible 2a; a nickel liquid holding and conveying mechanism is disposed on one side of the nickel liquid injection mechanism, used to hold and convey nickel liquid to the nickel liquid injection mechanism; a gas charging and discharging system includes a gas charging pipe 6 and a gas exhaust pipe 7, the gas outlet of the gas charging pipe 6 and the gas inlet of the gas exhaust pipe 7 are both disposed above the inner cavity of the furnace body. Wherein:

[0085] The heat insulation pad 1g is made of high-temperature cement material, and the base 1e is made of stainless steel material;

[0086] The crucible 2a is made of graphite clay material;

[0087] The spacer block 2d is made of graphite clay and is cylindrical with a diameter of 40mm and a height of 50mm.

[0088] The top surface of the upper perforated plate 2b is an arc surface, and the bottom surface of the upper perforated plate 2b is a plane. The edge thickness of the upper perforated plate 2b is 35mm, and the middle thickness is 25mm. There are six through holes 2b1 with a diameter of 10mm evenly distributed at a position 30mm away from the center on the upper perforated plate 2b. Each through hole 2b1 consists of one vertical hole 2b11 and two oblique holes 2b12. The vertical hole 2b11 is on top, and the oblique holes 2b12 are on the bottom. The angle between the axis of the oblique hole 2b12 and the axis of the vertical hole 2b11 is 45°.

[0089] The lower perforated plate 2c is made of graphite clay material and has a thickness of 25mm. It has six through holes 2c1, each with a diameter of 10mm. Each through hole 2c1 consists of one vertical hole 2c11 and two oblique holes 2c12, with the vertical hole 2c11 on top and the oblique holes 2c12 on the bottom. The angle between the axis of the oblique hole 2c12 and the axis of the vertical hole 2c11 is 45°. The vertical hole 2c11 on the through holes 2c1 is positioned 30mm from the edge of the lower perforated plate 2c.

[0090] The vertical hole 2b11 on the through hole 2b1 on the upper perforated plate 2b and the vertical hole 2c11 on the through hole 2c1 on the lower perforated plate 2c are not on the same axis.

[0091] The pressure cover mechanism 3 includes a pressure cover plate 3a, a pressure rod 3b, and a lifting mechanism 3c. The lower end of the pressure rod 3b is connected to the pressure cover plate 3a, and the upper end of the pressure rod 3b is connected to the lifting mechanism 3c. The bottom of the pressure cover plate 3a is provided with a foot 3a1, and the pressure cover plate 3a is connected to the upper orifice plate 2b of the double-stage throttling orifice plate assembly through the foot 3a1. The lifting mechanism 3c is located above the furnace cover 1b of the medium-frequency furnace 1, and the lifting mechanism 3c presses down on the upper orifice plate 2b through the pressure rod 3b and the pressure cover plate 3a. The pressure rod 3b and the pressure cover plate 3a are made of graphite clay material.

[0092] The nickel liquid injection mechanism is a funnel 4, which is made of graphite clay material;

[0093] The gas filling and exhaust system includes a filling pipe 6 and an exhaust pipe 7. The outlet of the filling pipe 6 is located above the inner cavity of the furnace body 1a, and the inlet of the filling pipe 6 is connected to a nitrogen source. The nitrogen source can be a nitrogen cylinder, nitrogen tank, or nitrogen generator. A filling valve 6a is provided on the filling pipe 6. The inlet of the exhaust pipe 7 is located above the inner cavity of the furnace body 1a, and the outlet of the exhaust pipe 7 is connected to a smoke removal device.

[0094] The nickel liquid holding and transporting mechanism is a ladle 5 made of graphite clay material.

[0095] The above description is merely a preferred embodiment of the present invention, but it should not be construed as limiting the scope of the present invention. Any simple equivalent changes and modifications made in accordance with the scope of the patent application and the description of the invention shall still fall within the scope of the patent of the present invention.

Claims

1. An apparatus for preparing a nickel-phosphorus master alloy, characterized in that, The apparatus for preparing the nickel-phosphorus master alloy includes an intermediate frequency furnace, a crucible assembly, a capping mechanism, a nickel liquid injection mechanism, a nickel liquid holding and conveying mechanism, a gas filling and discharging system, a lifting device, and a fixing frame. The intermediate frequency furnace includes a furnace body, a furnace cover, and a base. The furnace body and the base are separate structures. The furnace body is fixed on the fixing frame. A sealing ring is provided between the base and the furnace body. An upper heating coil and a lower heating coil are arranged on the inner wall of the furnace body in a top-to-bottom order. A heat insulation pad is provided on the top surface of the base. The base is located on top of the lifting device, which is placed on the ground. The crucible assembly includes a crucible and a two-stage throttling orifice plate assembly. The two-stage throttling orifice plate assembly includes an upper orifice plate, a lower orifice plate, and three or more spacer blocks. The spacer blocks are evenly distributed between the upper and lower orifice plates. The two-stage throttling orifice plate assembly cooperates with the crucible. The pressure cap mechanism is disposed above the crucible assembly and is used to press down the upper orifice plate of the two-stage throttling orifice plate assembly; The nickel liquid injection mechanism is located above the intermediate frequency furnace and is used to inject nickel liquid into the crucible; The nickel liquid holding and transporting mechanism is located on one side of the nickel liquid injection mechanism and is used to hold and transport nickel liquid to the nickel liquid injection mechanism; The gas filling and exhaust system includes a filling pipe and an exhaust pipe, with the outlet of the filling pipe and the inlet of the exhaust pipe both located above the inner cavity of the furnace body.

2. The apparatus for preparing a nickel-phosphorus master alloy according to claim 1, characterized in that, The base is made of stainless steel, the heat insulation pad is made of high-temperature cement, the crucible is made of graphite clay, the spacer is made of graphite clay and is cylindrical with a diameter of 10-50 mm and a height of 30-80 mm, the nickel liquid injection mechanism is a funnel made of graphite clay, and the nickel liquid holding and transporting mechanism is a ladle made of graphite clay.

3. The apparatus for preparing a nickel-phosphorus master alloy according to claim 1 or 2, characterized in that, The upper perforated plate is made of graphite clay material. The edge thickness of the upper perforated plate is 13-35 mm, and the middle thickness is 10-30 mm. The edge of the upper perforated plate can fit against the inner wall of the crucible. The top surface of the upper perforated plate is an arc surface, and the bottom surface of the upper perforated plate is a plane. One or more through holes are provided on the upper perforated plate. Each through hole consists of one vertical hole and one to three oblique holes. The vertical hole is on top, and the oblique holes are on the bottom. The angle between the axis of the oblique hole and the axis of the vertical hole is 30° to 60°. The diameter of the through hole is 3-15 mm.

4. The apparatus for preparing a nickel-phosphorus master alloy according to claim 1 or 2, characterized in that, The lower perforated plate is made of graphite clay material and has a thickness of 10-30 mm. One or more through holes are provided on the lower perforated plate. Each through hole consists of one vertical hole and one to three oblique holes, with the vertical hole at the top and the oblique holes at the bottom. The angle between the axis of the oblique hole and the axis of the vertical hole is 30°-60°. The diameter of the through hole is 3-15 mm.

5. The apparatus for preparing a nickel-phosphorus master alloy according to claim 1 or 2, characterized in that, The pressure cap mechanism includes a pressure cap plate, a pressure rod, and a lifting mechanism. The lower end of the pressure rod is connected to the pressure cap plate, and the upper end of the pressure rod is connected to the lifting mechanism. The bottom of the pressure cap plate is provided with a foot, and the pressure cap plate is connected to the upper orifice plate of the dual-stage throttling orifice plate assembly through the foot. The lifting mechanism is located above the furnace cover of the medium-frequency furnace. The lifting mechanism presses down on the upper orifice plate through the pressure rod and the pressure cap plate. The pressure rod and the pressure cap plate are made of graphite clay material.

6. The apparatus for preparing a nickel-phosphorus master alloy according to claim 1 or 2, characterized in that, The gas filling and exhaust system includes a filling pipe and an exhaust pipe. The outlet of the filling pipe is located above the inner cavity of the furnace body, and the inlet of the filling pipe is connected to a nitrogen source, which can be a nitrogen cylinder, nitrogen tank, or nitrogen generator. A filling valve is provided on the filling pipe. The inlet of the exhaust pipe is located above the inner cavity of the furnace body, and the outlet of the exhaust pipe is connected to a smoke removal device.

7. A process for preparing a nickel-phosphorus master alloy, characterized in that, The process employs the nickel-phosphorus master alloy preparation apparatus as described in claim 1, and specifically includes the following steps: (1) Weigh red phosphorus and electrolytic nickel according to the proportions; (2) Melt the weighed nickel blocks into liquid nickel and place them in a ladle for later use; (3) Place the weighed red phosphorus into the crucible and level it; (4) Cover the red phosphorus in the crucible with the lower perforated plate; (5) Place several spacer blocks evenly along the top edge of the lower perforated plate, and place the upper perforated plate on the spacer blocks; (6) Turn on the lowering switch of the lifting device. After the base descends to the lower stop position, place the crucible on the heat insulation pad on the base. Then turn on the raising switch of the lifting device. The base moves upward and sends the crucible into the cavity of the medium frequency furnace body. The upper hole plate is pressed by the pressure rod and pressure plate cover in the lifting mechanism located above the furnace cover of the medium frequency furnace. (7) Open the gas filling valve on the gas filling pipe and inject high-purity nitrogen into the furnace cavity of the medium frequency furnace. Then turn on the power switch of the upper heating coil to heat it. (8) After the temperature inside the furnace cavity of the medium frequency furnace rises to the set temperature, turn off the power switch of the upper heating coil to stop heating, and then pour the molten nickel in the ladle into the crucible inside the furnace cavity of the medium frequency furnace through the funnel. At the same time, the molten nickel entering the crucible flows into the red phosphorus through the through hole one on the upper plate and the through hole two on the lower plate and is mixed and melted. (9) After the molten nickel in the ladle is poured into the crucible inside the furnace cavity of the medium frequency furnace through the funnel, the power switches of the upper heating coil and the lower heating coil are turned on to start heating. At this time, the medium frequency furnace is in the state of smelting nickel-phosphorus intermediate alloy. During the smelting of nickel-phosphorus intermediate alloy, due to the low density of red phosphorus and the high density of molten nickel, red phosphorus will overflow upward through the through hole 2 of the lower orifice plate and the through hole 1 of the upper orifice plate, while molten nickel will enter the bottom of the crucible through the through hole 1 of the upper orifice plate and the through hole 2 of the lower orifice plate, so that red phosphorus and molten nickel gradually mix and melt. Turning on the power switches of the upper heating coil and the lower heating coil will stir the molten nickel in the crucible, so that red phosphorus will gradually mix and melt into the molten nickel. If flue gas is generated during the smelting of nickel-phosphorus intermediate alloy, the flue gas will be discharged to the smoke removal equipment for treatment through the exhaust pipe. (10) After the red phosphorus and nickel liquid are fully mixed and melted, the pressure rod and pressure plate cover are moved up by the lifting mechanism. The upper orifice plate, lower orifice plate and spacer block will float to the surface of the melt. Continue smelting for 3 to 10 minutes to make the melt composition uniform. (11) Turn off the power switches of the upper heating coil and the lower heating coil, close the gas filling valve, turn on the lowering switch of the lifting device, and after the base is lowered to the lower stop position, move the crucible out of the furnace cavity of the medium frequency furnace. Transfer the crucible to the casting mold edge through the crucible transfer device, use special tools to clamp out the upper hole plate, lower hole plate and spacer block, and finally cast the nickel-phosphorus intermediate alloy melt in the crucible to obtain the nickel-phosphorus alloy product.

8. The preparation process of a nickel-phosphorus master alloy according to claim 7, characterized in that, In step (1), the nickel used is electrolytic nickel, and the ratio between red phosphorus and electrolytic nickel is determined by mass percentage, wherein the mass percentage of red phosphorus is 0.5 to 20.0%, and the mass percentage of electrolytic nickel is 80.0 to 99.5%.

9. The preparation process of a nickel-phosphorus master alloy according to claim 7, characterized in that, In step (8), the temperature of the nickel liquid is 1600℃~1800℃.

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