CN112176206A

CN112176206A - Rectification purification device and method for preparing beryllium by beryllium fluoride by using rectification purification device

Info

Publication number: CN112176206A
Application number: CN202010996700.6A
Authority: CN
Inventors: 行卫东; 李清宇; 朱刘
Original assignee: Vital Materials Co Ltd
Current assignee: Vital Materials Co Ltd
Priority date: 2020-09-21
Filing date: 2020-09-21
Publication date: 2021-01-05
Anticipated expiration: 2040-09-21
Also published as: CN112176206B

Abstract

The invention provides a rectification and purification device and a method for preparing beryllium by beryllium fluoride by using the same, wherein the rectification and purification device comprises a reaction tube, a vacuum pumping device, a crucible, an induction coil, a condensation tube cover and a control power supply; the inner cavity of the condenser pipe is in a round table shape with the inner diameter being small at the top and big at the bottom. The method comprises the following steps: taking out the crucible and the condenser tube, placing beryllium fluoride and magnesium at the sealed bottom end of the reaction tube, starting a vacuumizing device for vacuumizing, and then electrifying the induction coil to heat the induction coil so as to perform a reduction reaction on the beryllium fluoride; washing the obtained beryllium with water and acid, tabletting, washing with acid and water, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser tube back into the device, starting a vacuumizing device to vacuumize, then electrifying an induction coil to heat the induction coil, and purifying the beryllium; and (4) cooling after purification is finished, taking beryllium distributed in the middle of the condensing tube, and carrying out acid washing, water washing and drying on the beryllium to obtain a final beryllium product.

Description

Rectification purification device and method for preparing beryllium by beryllium fluoride by using rectification purification device

Technical Field

The disclosure relates to the field of high-purity beryllium preparation, in particular to a rectification and purification device and a method for preparing beryllium through beryllium fluoride by using the rectification and purification device.

Background

Metallic beryllium is an irreplaceable strategic metal material in the fields of aviation, aerospace, war industry, electronics, nuclear energy and the like, and the purity of metallic beryllium determines various properties of the material. At present, the high-purity beryllium makes important progress in the research and development of new materials, and the preparation process mainly comprises the following methods: melting electrolysis, pyrolysis of beryllium hydride, vacuum distillation, alkali metal reduction and other process methods.

Patent publication No. CN109295309A reports a method for preparing metallic beryllium by reducing beryllium chloride, wherein gaseous beryllium chloride with purity of more than 70% is reduced by sodium metal under vacuum at 500-600 ℃, the mixture is purified by multi-stage distillation to recover metallic beryllium, the temperature is 960-1250 ℃, the pressure is 0.001-0.005 MPa, the purity of the obtained beryllium is 99.9%, and the recovery rate is more than 98%.

Zhang jiqiiang et al, 2017, in Powder technology 321, reported the preparation of ultrapure beryllium metal using a process for the pyrolysis of di-tert-butyl beryllium ether. The process adopts 5N high-purity di-tert-butyl beryllium ether, prepares high-purity beryllium hydride by heating and distilling in a glove box at the temperature of 200 ℃, and prepares 4N + high-purity beryllium metal by thermally decomposing the beryllium hydride.

In 1962, a method for preparing high-purity beryllium by molten salt electrolysis was reported in U.S. Pat. No. 3296107, wherein beryllium chloride is purified by vacuum distillation, and then mixed with sodium chloride or potassium chloride salt to be subjected to molten salt electrolysis in a nickel crucible, the temperature is controlled to be 300-400 ℃, the voltage is 1.95-2.5V, and the current density is 5mA/cm²-30mA/cm²The nickel crucible is used as a cathode, the graphite rod is used as an anode, and the metal beryllium with the purity of 99.9 percent is obtained.

However, the above process has high requirements for equipment and investment, and also has severe requirements for storage of raw materials such as beryllium chloride and 5N di-tert-butyl beryllium ether.

The above description is merely provided as background and is not an admission that the above "background" constitutes prior art to the present disclosure.

Disclosure of Invention

In view of the problems in the background art, the present disclosure provides a rectification purification apparatus and a method for preparing beryllium by beryllium fluoride using the same.

In one embodiment, the rectification and purification device disclosed by the disclosure comprises a reaction tube, a vacuum pumping device, a crucible, an induction coil, a condensation tube cover and a control power supply; the axial bottom end of the reaction tube is sealed and the axial top end is open; the vacuumizing device is hermetically connected with the top end of the reaction tube; the crucible is arranged in the reaction tube and supported at the bottom end of the reaction tube; the induction coil is sleeved outside the reaction tube and is positioned in the axial height range of the crucible; the control power supply is connected with the induction coil to control the heating of the induction coil; the condensation pipe is arranged in the reaction pipe and is axially positioned above the crucible, the inner cavity of the condensation pipe is communicated with the opening of the crucible, and the inner cavity of the condensation pipe is in a circular truncated cone shape with a small inner diameter at the top and a large inner diameter at the bottom; the condenser pipe cover covers the condenser pipe along the axial direction and is provided with a through hole which is communicated along the axial direction, and the through hole is communicated with the inner cavity of the condenser pipe.

In one embodiment, a method for producing beryllium by beryllium fluoride using the rectification purification apparatus of the present disclosure comprises the steps of: a. taking out the crucible and the condenser tube in the device, placing beryllium fluoride and magnesium at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize, and then electrifying the induction coil to heat the induction coil so as to cause the beryllium fluoride to perform a reduction reaction; b. b, washing beryllium obtained in the step a with water and acid, tabletting, washing with acid and water, and drying; c. b, placing the beryllium obtained by drying in the step b into a crucible, then putting the crucible and a condenser tube back into the device, starting a vacuumizing device to vacuumize, then electrifying an induction coil to heat the induction coil, and purifying the beryllium; d. and (4) cooling after purification is finished, taking beryllium distributed in the middle of the condensing tube, and carrying out acid washing, water washing and drying on the beryllium to obtain a final beryllium product.

The beneficial effects of this disclosure are as follows:

the rectification and purification device disclosed by the invention is simple and easy to operate; the method can effectively reduce the reduction temperature in the reduction process of the beryllium fluoride, and reduce the oxidation of magnesium and the oxidation of reduced beryllium in the reduction process; in addition, the purity of the finally obtained beryllium product reaches 99.95-99.995%, and the rectified residue can be recycled by adopting a wet process.

Drawings

FIG. 1 is a schematic view of an embodiment of the purification apparatus of the present disclosure, wherein the reaction tube is shown in a transparent state.

FIG. 2 is a cut-away view of FIG. 1, in which the reaction tube is shown in a transparent state.

Wherein the reference numerals are as follows:

100 rectification purification device

1 vacuum-pumping device

2 refractory material

3 external thermal insulation material

4 internal thermal insulation material

5 condenser tube cover

6 induction coil

7 crucible

O opening

71 graphite crucible

72 beryllium oxide crucible

8 condenser tube

S inner cavity

81 graphite hollow body

82 metal liner

9 reaction tube

10 reaction tube cover

10a fitting seal groove

10b perforation

11 control power supply

12 connecting pipe

Detailed Description

It is to be understood that the disclosed embodiments are merely exemplary of the disclosure that may be embodied in various forms, and that specific details of the disclosure are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the disclosure.

In the description of the present disclosure, terms and terms not explicitly described are common general knowledge of those skilled in the art, and methods not explicitly described are conventional methods known to those skilled in the art.

In the description of the present disclosure, unless otherwise specified or indicated, the term "connected" is to be understood broadly, for example, "connected" may be a fixed connection, a detachable connection, or an integrated connection, and "connected" may be a direct connection or an indirect connection through an intermediate medium. The specific meaning of the above terms in the present disclosure can be understood by those of ordinary skill in the art as appropriate.

In the description of the present disclosure, it should be understood that the terms "upper" and "lower" used in the embodiments of the present disclosure are used in a descriptive sense only and not for purposes of limitation. The present disclosure is described in further detail below with reference to specific embodiments and with reference to the attached drawings.

In one embodiment, as shown in fig. 1 and 2, the rectification and purification apparatus 100 of the present disclosure comprises a reaction tube 9, a vacuum extractor 1, a crucible 7, an induction coil 6, a condensation tube 8, a condensation tube cover 5, and a control power source 11. Wherein, the axial bottom end of the reaction tube 9 is sealed and the axial top end is open; the vacuumizing device 1 is hermetically connected with the top end of the reaction tube 9; the crucible 7 is arranged in the reaction tube 9 and supported at the bottom end of the reaction tube 9; the induction coil 6 is sleeved outside the reaction tube 9 and is positioned in the axial height range of the crucible 7; the control power supply 11 is connected to the induction coil 6 to control heating of the induction coil 6; the condensation pipe 8 is provided with openings at two axial ends, the condensation pipe 8 is arranged in the reaction pipe 9 and is positioned above the crucible 7 along the axial direction, an inner cavity S of the condensation pipe 8 is communicated with the opening O of the crucible 7, and the inner cavity S of the condensation pipe 8 is in a circular truncated cone shape with a small inner diameter at the top and a large inner diameter at the bottom; the condenser cover 5 is axially covered on the condenser pipe 8 and has a through hole 51 penetrating in the axial direction, and the through hole 51 communicates with the inner cavity S of the condenser pipe 5.

In one embodiment, the distillation purification apparatus 100 further comprises an outer insulation material 3, a refractory material 2, and an inner insulation material 4.

In one embodiment, the outer insulating material 3 surrounds the reaction tube 9 from the outside and covers at least the position of the crucible 7 and a part of the condensation tube 8 in the axial direction. In some embodiments, the outer insulating material 3 includes at least one of carbon felt and insulating cotton.

In one embodiment, the refractory material 2 externally surrounds the insulating material 3. In one embodiment, the refractory material 2 comprises refractory bricks. As shown, the refractory material 2 and the outer insulating material 3 are each two segments axially spaced apart to facilitate installation and removal of the induction coil 6.

In one embodiment, the inner insulating material 4 is located inside the reaction tube 9 and surrounds at least a part of the crucible 7 and the condenser tube 8 from the outside in the axial direction, thereby not only performing an insulating function but also simultaneously performing a function of fixing the crucible 7 and the condenser tube 8. In some embodiments, the inner insulating material 4 comprises at least one of carbon felt, insulating cotton. In the present disclosure, the temperature stability and the temperature control precision of the condenser pipe 8 during operation can be fully ensured by the inner thermal insulation material 4, the outer thermal insulation material 3 and the refractory material 2, and the accuracy of the condenser pipe 8 during distillation and purification is improved.

In one embodiment, the distillation purification apparatus 100 further comprises a quartz tube cover 10. The quartz tube cover 10 has a fitting seal groove 10a and a through hole 10b, and the fitting seal groove 10a receives and seals the axial tip of the reaction tube 9. The fitting seal groove 10a not only enables sealing but also enables the quartz tube cap 10 to be detachable.

In one embodiment, the vacuum apparatus 1 communicates with the inside of the reaction tube 9 through the connection tube 12 and the through hole 10b of the quartz tube cover 10. In one embodiment, the material of the connecting tube 12 includes quartz.

In one embodiment, crucible 7 comprises a graphite crucible 71 and a beryllium oxide crucible 72 embedded within graphite crucible 71. In some embodiments, the material of the crucible 7 includes at least one of graphite and beryllium oxide.

In one embodiment, the condenser tube 8 includes a graphite hollow body 81 and a metal liner 82. In one embodiment, the material of the condenser tube 8 includes graphite with a purity of 5N-5N 5.

In an embodiment, the present disclosure further provides a method for preparing beryllium by beryllium fluoride by using the rectification and purification apparatus of the present disclosure, including the steps of:

a. taking out the crucible 7 and the condenser tube 8 in the device, placing beryllium fluoride and magnesium at the sealed bottom end of the reaction tube 9, starting the vacuumizing device 1 to vacuumize, and then electrifying the induction coil 6 to heat the induction coil so as to reduce the beryllium fluoride;

b. b, washing beryllium obtained in the step a with water and acid, tabletting, washing with acid and water, and drying;

c. b, placing the beryllium dried in the step b in a crucible, then putting the crucible 7 and the condenser pipe 8 back into the device, starting the vacuumizing device 1 to vacuumize, then electrifying the induction coil 6 to heat the induction coil, and purifying the beryllium;

d. and (4) cooling after purification is finished, taking beryllium distributed in the middle of the condensing tube, and carrying out acid washing, water washing and drying on the beryllium to obtain a final beryllium product.

In some embodiments, in step a, the purity of beryllium fluoride is greater than 99.99% and the purity of magnesium is greater than 99.99% in parts by weight.

In some embodiments, in step a, the vacuum degree is 5Pa to 10Pa, and the current of the induction coil 6 is 50A to 55A.

In some embodiments, in step b, the water washing is performed by deionized water, and the acid washing is performed by one or more of sulfuric acid, nitric acid, hydrochloric acid, and hydrofluoric acid.

In some embodiments, in step c, the vacuum degree is 2Pa-6 Pa, and the current of the induction coil 6 is 50A-55A.

In some embodiments, in step d, the acid cleaning is performed by alternately cleaning with one or two of nitric acid and hydrofluoric acid.

The disclosure is further illustrated with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure.

In the following examples and comparative examples, reagents, materials and instruments used were commercially available or prepared by methods known in the art, unless otherwise specified.

Example 1

Taking out a crucible and a condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of a reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying an induction coil to ensure that the current of the coil is controlled to be 55A to heat a reactant so as to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser tube back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 2Pa, then electrifying an induction coil to control the current of the coil to be 55A to heat the beryllium in the crucible, and purifying the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

Example 2

Taking out a crucible and a condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of a reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 10Pa, and then electrifying an induction coil to ensure that the current of the coil is controlled to be 50A to heat a reactant so as to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with hydrofluoric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser tube back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 6Pa, then electrifying an induction coil to control the current of the coil to be 50A to heat the beryllium in the crucible, and purifying the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

Example 3

Taking out the crucible and the condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize to make the vacuum degree be 8Pa, and then electrifying the induction coil to control the current of the coil to be 54A to heat the reactants so as to make the beryllium fluoride undergo a reduction reaction; washing the obtained beryllium beads with water, treating with hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser tube back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to make the vacuum degree be 4Pa, then electrifying an induction coil to control the current of the coil to be 53A to heat the beryllium in the crucible, and purifying the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, and obtaining a final beryllium product after hydrofluoric acid treatment, water washing, neutralization and drying.

Example 4

Taking out the crucible and the condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 6Pa, and then electrifying the induction coil to ensure that the current of the coil is controlled to be 53A to heat the reactant to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser tube back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, then electrifying an induction coil to ensure that the current of the coil is controlled to be 54A to heat the beryllium in the crucible, and purifying the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

Example 5

Taking out the crucible and the condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying the induction coil to ensure that the current of the coil is controlled to be 53A to heat the reactant to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condenser pipe lined with a tantalum sheet back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying an induction coil to ensure that the current of the coil is controlled to be 54A to heat the beryllium in the crucible to purify the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

Example 6

Taking out the crucible and the condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 6Pa, and then electrifying the induction coil to ensure that the current of the coil is controlled to be 53A to heat the reactant to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the dried beryllium in a crucible, then putting the crucible and a condensing tube lined with a titanium sheet back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying an induction coil to ensure that the current of the coil is controlled to be 54A to heat the beryllium in the crucible to purify the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

Example 7

Taking out the crucible and the condenser tube in the device shown in FIG. 1, placing magnesium and 50g of beryllium fluoride with the purity of 99.99% at the sealed bottom end of the reaction tube, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying the induction coil to ensure that the current of the coil is controlled to be 53A to heat the reactant to ensure that the beryllium fluoride undergoes a reduction reaction; washing the obtained beryllium beads with water, treating with nitric acid and hydrofluoric acid, tabletting, treating with nitric acid, washing with water to neutralize, and drying; placing the beryllium obtained by drying in a crucible, then putting the crucible and a condensation pipe lined with a Mo sheet back into the device in the embodiment 1, starting a vacuumizing device to vacuumize to ensure that the vacuum degree is 5Pa, and then electrifying an induction coil to ensure that the current of the coil is controlled to be 54A to heat the beryllium in the crucible, so as to purify the beryllium; and (4) cooling after purification is finished, taking beryllium in the middle of the condensing tube, treating the beryllium by nitric acid and hydrofluoric acid, washing the beryllium with water to be neutral, and drying the beryllium to obtain a final beryllium product.

The procedure for testing the purity and impurity content of the final beryllium product is described below.

The beryllium product was tested for purity by Glow Discharge Mass Spectrometry (GDMS): and (3) etching 7N indium cleanly by using acid, pressing the indium into a sheet with the diameter of about 15mm, etching the indium cleanly by using acid again, drying the indium in a clean bench, covering the beryllium sample on the weighing paper by using the indium, pressing the indium until the beryllium sample is adhered to the indium sheet and does not fall off, putting the indium wrapping the beryllium sample on a sheet sample rack, and then adjusting related parameters of a GDMS glow discharge instrument and carrying out data acquisition.

The test results of examples 1-7 are shown in Table 1.

TABLE 1

From the preparation and test results of examples 1-7, it can be seen that the beryllium is purified by reduction of beryllium fluoride using the rectification and purification device of the present disclosure, the purity of the final beryllium product is as high as 99.95% -99.995%, and the impurity content in the final beryllium product is low.

In addition, the beryllium residues existing at the upper end and the lower end of the condensation pipe after rectification can be recycled by adopting a wet process.

Claims

1. A rectification purification device is characterized by comprising a reaction tube (9), a vacuumizing device (1), a crucible (7), an induction coil (6), a condensation tube (8), a condensation tube cover (5) and a control power supply (11);

the axial bottom end of the reaction tube (9) is sealed and the axial top end is open;

the vacuumizing device (1) is hermetically connected with the top end of the reaction tube (9);

the crucible (7) is arranged in the reaction tube (9) and supported at the bottom end of the reaction tube (9);

the induction coil (6) is sleeved outside the reaction tube (9) and is positioned in the axial height range of the crucible (7);

the control power supply (11) is connected with the induction coil (6) to control the heating of the induction coil (6);

the two axial ends of the condenser tube (8) are opened, the condenser tube (8) is arranged in the reaction tube (9) and is positioned above the crucible (7) along the axial direction, the inner cavity (S) of the condenser tube (8) is communicated with the opening (O) of the crucible (7), the inner cavity (S) of the condenser tube (8) is in a round table shape with the inner diameter being small at the top and big at the bottom,

the condenser pipe cover (5) is covered on the condenser pipe (8) along the axial direction and is provided with a through hole (51) which is through along the axial direction, and the through hole (51) is communicated with the inner cavity (S) of the condenser pipe (5).

2. The rectification purification apparatus according to claim 1,

the rectification and purification device (100) also comprises an external thermal insulation material (3), a refractory material (2) and an internal thermal insulation material (4);

the outer heat insulating material (3) surrounds the reaction tube (9) from the outside and covers the crucible (7) and a part of the condensation tube (8) at least along the axial direction;

the refractory material (2) surrounds the heat insulating material (3) from the outside;

the inner heat insulating material (4) is located in the reaction tube (9) and surrounds the crucible (7) and a part of the condensation tube (8) from the outside at least in the axial direction.

3. The rectification purification apparatus according to claim 1,

the rectification and purification device (100) further comprises a quartz tube cover (10), wherein the quartz tube cover (10) is provided with a chimeric sealing groove (10a) and a through hole (10b), and the chimeric sealing groove (10a) accommodates and seals the axial top end of the reaction tube (9);

the vacuum extractor (1) is communicated with the inside of the reaction tube (9) through a connecting tube (12) and a perforation (10b) of the quartz tube cover (10).

4. Rectification purification device according to claim 1, characterized in that the crucible (7) comprises a graphite crucible (71) and a beryllium oxide crucible (72) embedded in the graphite crucible (71).

5. Rectification purification device according to claim 1, characterized in that the condensation duct (8) comprises an ink hollow body (81) and a metal lining (82).

6. A method for producing beryllium by beryllium fluoride using the rectification purification device of any one of claims 1 to 5, comprising the steps of:

a. taking out a crucible (7) and a condenser tube (8) in the device, placing beryllium fluoride and magnesium at the sealed bottom end of a reaction tube (9), starting a vacuumizing device (1) for vacuumizing, and then electrifying an induction coil (6) to heat the induction coil to ensure that the beryllium fluoride is subjected to a reduction reaction;

c. b, placing the beryllium obtained by drying in the step b into a crucible, then putting the crucible (7) and a condensing tube (8) back into the device, starting a vacuumizing device (1) for vacuumizing, then electrifying an induction coil (6) to heat the induction coil, and purifying the beryllium;

7. The method for preparing beryllium through beryllium fluoride according to claim 6, wherein in the step a, the purity of beryllium fluoride is more than 99.99 percent and the purity of magnesium is more than 99.99 percent in parts by weight; the vacuum degree of the vacuum pumping is 5Pa-10Pa, and the current electrified in the induction coil (6) is 50A-55A.

8. The method for preparing beryllium through beryllium fluoride according to claim 6, wherein in the step b, the water washing is performed by using deionized water, and the acid washing is performed by using one or more of sulfuric acid, nitric acid, hydrochloric acid and hydrofluoric acid.

9. The method for preparing beryllium through beryllium fluoride according to claim 6, wherein in step c, the vacuum degree is 2Pa to 6Pa, and the current for electrifying the induction coil (6) is 50A to 55A.

10. The method for preparing beryllium through beryllium fluoride according to claim 6, wherein in the step d, the acid washing is alternately cleaned by one or a mixture of nitric acid and hydrofluoric acid.