阅读说明：本技术 一种制备高纯单质金属的工艺 (Process for preparing high-purity elemental metal ) 是由 韩坦 朱戴博 王富涛 陈�峰 刘洪涛 陈红 于 2020-07-13 设计创作，主要内容包括：本发明提出的一种制备高纯单质金属的工艺,它包括：安装重熔装置,投料,旋转并熔融、旋转冷并却,截除等工序,方法利用液体金属遇到离心力后密度会变化的原理,在金属熔化时旋转臂筒产生离心力,可以使臂筒内的液态金属的自身密度达到原来的10倍～20倍以上,使气体向上浮起,有效分离液体单质金属中的气体,夹在在液体金属中的重金属在臂筒旋转时,被甩向臂筒的两端提高了单质金属的纯度,通过将该装置置于真空罩,有效防止单质金属被氧化的问题发生,在熔体旋转时通入液氮,液氮预热成为氮气,臂筒在旋转时降温,使臂筒内的液体金属凝固,工作效率高。(The invention provides a process for preparing high-purity elemental metal, which comprises the following steps: the method utilizes the principle that the density of liquid metal can change after encountering centrifugal force, the rotating arm cylinder generates centrifugal force when the metal is molten, the density of the liquid metal in the arm cylinder can reach more than 10-20 times of the original density, the gas is enabled to float upwards, the gas in the liquid elemental metal is effectively separated, the purity of the elemental metal is improved when heavy metal clamped in the liquid metal is thrown to two ends of the arm cylinder when the arm cylinder rotates, the device is placed in a vacuum cover, the problem that the elemental metal is oxidized is effectively prevented, liquid nitrogen is introduced when a melt rotates and is preheated to be nitrogen, the arm cylinder is cooled when rotating, the liquid metal in the arm cylinder is solidified, and the working efficiency is high.)

1. A process for preparing high purity elemental metal, comprising: the process comprises the following steps:

the remelting device is arranged on a desktop or a supporting plate, a hole for accommodating a water-cooling coaxial electric brush (17) is formed in the desktop or the supporting plate, and the water-cooling coaxial electric brush (17) is communicated with a medium-frequency power supply cabinet (172);

step two, taking down a vacuum cover (20) of the remelting device from a shell bottom plate (25), and throwing simple substance metal blanks into a storage barrel (100), wherein the simple substance metal blanks are filled in the tee joint (2), the arm cylinder (2) and the storage barrel (100);

step three, after the simple substance metal blank is put in, covering a vacuum cover (20) on a shell bottom plate (25), then sealing and installing the joint of the vacuum cover (20) and the shell bottom plate (25) through a sealing material, vacuumizing the vacuum cover (20), and then starting a vacuum motor (12) and an intermediate frequency power cabinet (172);

driving a transmission belt (191) to work by a vacuum motor (12), transmitting power to a gear pair (19) by the transmission belt (191), transmitting the power to a lower transmission block (11) penetrating through a gear by the gear pair (19), and driving a support plate (10) and a tee joint (2) and an arm cylinder bushing (4) which are fixedly arranged on the support plate (10) to rotate by the lower transmission block (11);

when the tee joint (2) and the arm cylinder bushing (4) rotate, the intermediate frequency power supply cabinet (172) heats the arm cylinder bushing (4) sleeved on the outer side of the arm cylinder (3) through the water-cooling coaxial electric brush (17) by the water-cooling coil (14);

fifthly, after the temperature in the tee joint (2) and the arm cylinder (3) is measured to reach a limit value by a temperature measuring gun (2002), the water-cooling coil (14) continuously heats the tee joint and the arm cylinder for 7-15 min, so that the elemental metal is melted; the supporting plate (10) drives the melt in the arm cylinder (3) to continuously rotate for 8-12 min to separate bubbles and heavy metal;

step six, after the water-cooling coil (14) is powered off, the time for inputting liquid nitrogen into the input port (201) on the vacuum cover (20) and the time for driving the arm cylinder (3) to rotate by the support plate (10) are both 6-18 min, and after the temperature in the tee joint (2) and the arm cylinder (3) reaches the room temperature measured by the temperature measuring gun (2002), the vacuum motor (12) stops working;

and step seven, opening a vacuum cover, taking the tee joint (2) down from the upper support block (15), vertically cutting along the outer diameter direction of the first end (21) of the tee joint (2) to obtain a remelting section (B) of the second end (22), the third end (23) and the first end (21) which are separated, vertically cutting half of the length of the end parts of the rest second end (22) and the rest third end (23) towards the original first end (21), cutting the end parts far away from the second end (22) and the third end (23) into a finished pure elemental metal billet (A), and cutting the end parts of the second end (22) and the third end (23) into the remelting section (B).

2. The process of claim 1, wherein the elemental metal is selected from the group consisting of: in the second step, the height h of the first end (21) of the tee joint (2) is less than or equal to the length L of the arm cylinder (3), and the diameter D of the first end (21) is more than or equal to 1.4 times of the diameter D of the arm cylinder (3).

3. The process of claim 2, wherein the elemental metal is selected from the group consisting of: in the second step, the apparent density of the elementary metal is 0.6g/cm³～0.7g/cm³The formula of the volume of the elementary metal filled in the storage barrel (100) is as follows: v_{Store up}＝πD²L, the diameter of the first end (21) is D, and the length of the arm cylinder (3) is L.

4. The process of claim 1, wherein the elemental metal is selected from the group consisting of: in the fourth step, the rotating speed of the supporting plate (10) is 300r/min to 600 r/min.

5. The process of claim 1, wherein the elemental metal is selected from the group consisting of: in the fifth step, the temperature of the limit value in the tee joint (2) and the arm cylinder (3) is 1300-1400 ℃.

6. The process of claim 1, wherein the elemental metal is selected from the group consisting of: the temperature measuring gun (2002), the vacuum motor (12) and the intermediate frequency power supply cabinet (172) are respectively connected with the PLC circuit.

The heating time of the water-cooling coil (14) is 7-15 min, the time for the support plate (10) to drive the melt in the arm cylinder (3) to continuously rotate is 8-12 min, and after the water-cooling coil (14) is powered off, the time for the input port (201) on the vacuum cover (20) to input liquid nitrogen and the time for the support plate (10) to drive the arm cylinder (3) to rotate are both 6-18 min.

7. The process of claim 1, wherein the elemental metal is selected from the group consisting of: the second end (22) and the third end (23) of the tee joint (2) are respectively in threaded connection with the end parts of the two arm cylinders (3).

8. The process of claim 1, wherein the elemental metal is selected from the group consisting of: arm section of thick bamboo bush (4) be connected with tee bend (2) interference fit, fire prevention buffer layer (5) and arm section of thick bamboo bush (4) internal surface counterbalance of establishing are overlapped to the arm section of thick bamboo (3) outside.

9. The process of claim 1, wherein the elemental metal is selected from the group consisting of: the arm cylinder bushing (4) is connected with a water-cooling coil (14) arranged on the outer side of the storage barrel bushing (1) through a wiring groove (24), and the water-cooling coil (14) on the arm cylinder bushing (4) is connected with a water-cooling coaxial electric brush (17) after penetrating through a supporting plate (10) and a wire transmission hole (18) on a lower transmission block (11) through the wiring groove (24).

10. The process of claim 1, wherein the elemental metal is selected from the group consisting of: the vacuum motor (12) is connected with the lower transmission block (11) through a gear pair (19) and a belt transmission (191).

Technical Field

The invention relates to the field of metal material processing, in particular to a process for preparing high-purity elemental metal.

Background

The simple substance metal is a pure substance composed of the same element, the simple substance metal must be a pure substance composed of one metal element, and therefore the mixture cannot be a simple substance. The simple substance metal is usually prepared by physical separation method, thermal decomposition method, reduction method, electrolysis method, oxidation method and other methods, however, in the prior art, the pure substance with the same element composition needs to be prepared, and various technical difficulties exist, for example, beryllium is increasingly regarded as a new material, and is an indispensable precious material in the atomic energy, rocket, missile, aviation, space navigation and metallurgical industry.

Although the application field of beryllium is very wide, in the prior art, if beryllium beads are directly melted into a beryllium ingot, the beryllium ingot is easy to melt in a vacuum state, a compact beryllium oxide film is easily formed on the surface of liquid beryllium due to the low density of the beryllium, and gas and metal impurities in the liquid beryllium cannot be removed and separated due to the light dead weight of the beryllium ingot, so that the finally obtained beryllium ingot is spongy even processed by a vacuum remelting mode, a large number of pores cannot be removed, and the metal impurities with high density are precipitated at the bottom.

Disclosure of Invention

The purpose of the invention is as follows: in order to solve the defects of the prior art, the process for preparing the high-purity elemental metal is simple, ensures the purity of the prepared elemental metal, has high efficiency of preparing the elemental metal, and effectively removes air holes and impurities of a metal ingot.

The technical scheme is as follows: in order to achieve the above object, the present invention provides a process for preparing a high purity elemental metal, comprising the steps of:

the remelting device is arranged on a tabletop or a supporting plate, a hole for accommodating a water-cooling coaxial electric brush is formed in the tabletop or the supporting plate, and the water-cooling coaxial electric brush is communicated with a medium-frequency power supply cabinet;

taking down a vacuum cover of the remelting device from a bottom plate of the shell, and putting simple substance metal blanks into the storage barrel, wherein the simple substance metal blanks are filled in the tee joint, the arm cylinder and the storage barrel;

step three, after the simple substance metal blank is put in, covering a vacuum cover on the bottom plate of the shell, then sealing and installing the joint of the vacuum cover and the bottom plate of the shell through a sealing material, vacuumizing the vacuum cover 20, and then starting a vacuum motor and a medium-frequency power supply cabinet;

driving a transmission belt to work by a vacuum motor, transmitting power to a gear pair by the transmission belt), transmitting the power to a lower transmission block penetrating through the gear by the gear pair, and driving a support plate, a tee joint and an arm cylinder bushing which are fixedly arranged on the support plate to rotate by the lower transmission block;

when the tee joint and the arm cylinder bushing rotate, the intermediate frequency power supply cabinet heats the arm cylinder bushing sleeved on the outer side of the arm cylinder through the water-cooling coaxial electric brush and the water-cooling coil;

fifthly, after the temperature in the tee joint and the arm cylinder is measured by the temperature measuring gun to reach a limit value, the water cooling coil continuously heats the tee joint and the arm cylinder for 7-15 min, so that the elemental metal is melted; the supporting plate drives the melt in the arm cylinder to continuously rotate for 8-12 min to separate bubbles and heavy metals;

step six, after the water-cooling coil is powered off, the time for inputting liquid nitrogen into the input port of the vacuum cover and the time for driving the arm cylinder to rotate by the support plate are both 6-18 min, and after the temperature in the tee joint and the arm cylinder is measured by the temperature measuring gun to reach the room temperature, the vacuum motor stops working;

and step seven, opening the vacuum cover, taking the tee joint off the upper support block, vertically cutting off the tee joint along the outer diameter direction of the first end of the tee joint to obtain a remelting section of the separated second end, third end and first end, vertically cutting off half of the length of the end of the rest second end 22 and third end 23 towards the original first end 21 direction, cutting off the end far away from the second end 22 and third end 23 to obtain a finished pure elemental metal billet, and cutting off the end of the second end 22 and third end 23 to obtain a remelting section.

As a further preferred of the invention, the temperature measuring gun sends a signal to the PLC circuit, and the PLC circuit controls the medium-frequency power cabinet and the vacuum motor to be switched on and off

Preferably, in the second step, the height h of the first end of the tee joint is less than or equal to the length L of the arm cylinder, and the diameter D of the first end is greater than or equal to 1.4 times of the diameter D of the arm cylinder, so that the equipment can be kept in balance in a high-speed and high-temperature working state, and the working stability of the equipment is ensured.

As a further preferred aspect of the present invention, in the second step, the bulk density of the elemental metal is 0.6g/cm³～0.7g/cm³The formula of the volume of the elementary metal filled in the storage barrel is as follows: v_{Store up}＝πD²And 2. L, the diameter of the first end is D, the length of the arm cylinder is L, the volume of the simple substance metal to be filled into the tee joint, the arm cylinder and the storage bucket is calculated according to the apparent density, and then the equipment is vacuumized, so that the equipment can be electrified to work.

As a further preferred aspect of the present invention, in the second step, the rotation speed of the supporting plate is 300r/min to 600r/min, and the data can keep the equipment balanced in a high-speed and high-temperature working state, so as to ensure the working stability of the equipment;

preferably, in the second step of the present invention, the temperature of the tee joint and the limiting value in the arm cylinder is 1300-1400 ℃, the arm cylinder rotates when the elemental metal is melted, and the self density of the liquid elemental metal in the arm cylinder can reach more than 20 times of the original density when the arm cylinder rotates, so as to effectively separate the gas in the liquid elemental metal and enable the gas to float upwards.

As a further preferred mode of the invention, the temperature measuring gun, the sensor on the supporting plate, the input port and the output port on the vacuum cover, the vacuum motor and the intermediate frequency power supply cabinet are respectively connected with the PLC circuit.

As a further preferable mode of the invention, the second end and the third end of the tee joint are respectively connected with the end parts of the two arm cylinders in a threaded mode.

As a further preferable mode of the invention, the arm cylinder bushing is connected with the tee joint in an interference fit manner, the fireproof buffer layer sleeved on the outer side of the arm cylinder abuts against the inner surface of the arm cylinder bushing, the fireproof buffer layer is high-zirconium aluminum silicate fiber cloth, a high-zirconium aluminum silicate plate or a high-zirconium aluminum silicate pipe, and the fireproof buffer layers are arranged on the outer side of the arm cylinder and the inner side of the arm cylinder bushing, so that the arm cylinder is effectively prevented from shaking in the arm cylinder bushing, the connection reliability and stability of the arm cylinder and the tee joint are improved, and the working efficiency of the equipment is ensured.

As a further optimization of the invention, the water-cooling coils arranged on the outer sides of the arm cylinder bushing and the storage bucket bushing are connected through the wiring groove, and the water-cooling coils on the arm cylinder bushing are connected with the water-cooling coaxial electric brush after penetrating through the wiring holes on the supporting plate and the lower transmission block through the wiring groove.

As a further preferred aspect of the present invention, the vacuum motor is connected to the lower transmission block through a gear pair and a belt transmission, one end of the lower transmission block is fixedly connected to the support plate, the end of the other end of the lower transmission block is mounted on a bearing seat, the bearing seat is fixed to a housing bottom plate hermetically connected to the vacuum cover, the vacuum cover is disposed above the housing bottom plate, and then the connection between the vacuum cover and the housing bottom plate is hermetically mounted through a sealing material;

in a further preferred embodiment of the present invention, the arm cylinder has an arm cylinder end plate at an outer end thereof, and the vacuum cover has an input port for inputting liquid nitrogen and an output port for discharging nitrogen gas.

As a further optimization of the invention, the lower surface of the tee joint is provided with a hole with internal threads, the position of the hole is opposite to that of the first end, the axial center position of the upper surface of the supporting plate is provided with an upper supporting block, the external threads arranged on the supporting block are matched and connected with the internal threads in the hole of the tee joint

As a further optimization of the invention, a bushing limiting plate which is close to the outer side of an arm cylinder end plate is fixed on an arm cylinder bushing and is connected with the limiting plate through a bolt, after two arm cylinders are respectively connected with a tee joint, the arm cylinders and the tee joint are axially fixed together to form a whole, and the bolt is connected with the limiting plate, so that the coaxiality of the connection of the tee joint and the arm cylinders is ensured, and the working stability of the equipment is further ensured.

As a further preferred embodiment of the present invention, the screw penetrates through the pressing strip to fix the water-cooling coil on the positioning plate, and since the positioning plate and the supporting plate are fixed together, when the water-cooling coil sleeved outside the arm cylinder bushing is fixed on the positioning plate, the radial fixation of the arm cylinder bushing, that is, the radial fixation of the arm cylinder, is realized.

Preferably, the heating time of the water-cooling coil is 7-15 min, so that the elemental metal blank is melted into liquid elemental metal, the support plate drives the arm cylinder to continuously rotate for 8-12 min, then air in the liquid elemental metal gradually floats to the top of the first end of the tee joint, heavy metals in the liquid elemental metal gradually accumulate towards two ends of the arm cylinder, after the water-cooling coil is powered off, the support plate continuously rotates to drive the arm cylinder to rotate, the time for inputting liquid nitrogen into the input port of the vacuum cover and the time for the support plate to drive the arm cylinder to rotate are 6-18 min, the liquid nitrogen is heated into nitrogen, the arm cylinder bushing and the arm cylinder are integrally cooled, and the liquid elemental metal in the arm cylinder is solidified into an elemental metal ingot blank.

As a further preferable mode of the invention, the material of the storage barrel bushing, the tee joint, the arm cylinder and the arm cylinder bushing is a high-purity graphite crucible, beryllium oxide ceramic or tungsten crucible.

As a further preferable mode of the present invention, the elemental metal blanks charged into the storage vat are beryllium beads, aluminum blanks, silver blanks, and other elemental metals with low density.

Has the advantages that: compared with the prior art, the process for preparing the high-purity elemental metal has the following advantages:

1. the method utilizes the principle that the density of liquid metal can change after encountering centrifugal force, and rotates the arm cylinder to generate centrifugal force when the metal is melted, so that the density of the liquid metal in the arm cylinder can reach more than 10-20 times of the original density, gas in the liquid simple substance metal is effectively separated, and the gas floats upwards;

2. heavy metals clamped in the liquid metals are thrown to two ends of the arm cylinder when the arm cylinder rotates, so that the heavy metals in the melt are effectively separated;

3. the device is arranged in the vacuum cover, so that the problem that elemental metal is oxidized is effectively prevented;

4. liquid nitrogen is introduced into the melt during rotation, the liquid nitrogen is preheated to become nitrogen, and the arm cylinder is cooled during rotation to solidify liquid metal in the arm cylinder.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is a top view of the present invention;

FIG. 3 is a partial view of the present invention;

FIG. 4 is a schematic view of a simple substance metal ingot.

Detailed Description

The invention is further elucidated with reference to the drawings and the embodiments.

As shown in fig. 1, fig. 2 and fig. 3, the process for preparing high-purity elemental metal according to the present invention obtains high-purity elemental metal by using a centrifugal remelting in-situ solidification device.

The centrifugal remelting in-situ solidification device comprises: the vacuum device comprises a tee joint 2 positioned in a vacuum cover 20, an inverted V-shaped storage barrel 100 sleeved at a first end 21 of the tee joint 2, a storage barrel lining 1 sleeved at the outer side of the storage barrel 100, arm cylinder linings 4 respectively sleeved at the outer sides of a second end 22 and a third end 23 of the tee joint 2, arm cylinders 3 respectively penetrated in the second end 22 and the third end 23, a supporting plate 10 for supporting the tee joint 2, a lower transmission block 11 positioned below the supporting plate 10 and a vacuum motor 12 positioned at one side of the transmission block 11, wherein the vacuum motor 12 is connected with the lower transmission block 11 through a gear pair 19 and a belt transmission 191;

one end of the lower transmission block 11 is fixedly connected with the support plate 10, the end part of the other end is installed on a bearing seat 171, and the bearing seat 171 is fixed on the shell bottom plate 25;

a wiring groove 24 is formed in the tee joint 2, a water-cooling coil 14 arranged on the outer sides of the material storage barrel bushing 1 and the arm cylinder bushing 4 is connected through the wiring groove 24, the water-cooling coil 14 on the arm cylinder bushing 4 penetrates through a supporting plate 10 and a wire transmission hole 18 on the lower transmission block 11 through the wiring groove 24 and then is connected with a water-cooling coaxial electric brush 17, the water-cooling coaxial electric brush 17 is connected to a medium-frequency power supply cabinet 172, the water-cooling coil 14 is fixedly connected with a positioning plate 9, and the positioning plate 9 is fixedly arranged above the supporting plate 10;

the outer side end of the arm cylinder 3 is provided with an arm cylinder end plate 6, and the vacuum cover 20 is provided with an input port 201 for inputting liquid nitrogen and an output port 202 for removing nitrogen.