CN109182786B - Method and device for preparing high-purity metal beryllium by volatilizing oxygen-free impurities - Google Patents
Method and device for preparing high-purity metal beryllium by volatilizing oxygen-free impurities Download PDFInfo
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- CN109182786B CN109182786B CN201811058307.1A CN201811058307A CN109182786B CN 109182786 B CN109182786 B CN 109182786B CN 201811058307 A CN201811058307 A CN 201811058307A CN 109182786 B CN109182786 B CN 109182786B
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Abstract
The invention discloses a refining method and a refining device of metal beryllium, wherein beryllium balls containing impurities are heated under the oxygen-free condition, the heating temperature is higher than the melting point of beryllium and the boiling point of the impurities, the beryllium balls are melted to form liquid drops which emerge from small holes on the side surface of an upper crucible and fall down, and in the dropping process, impurity elements are volatilized to obtain refined beryllium; the length of an adjustable bracket (8) of the raw material crucible is adjusted to change the volatilization time; a crucible with an opening on the side wall and an adjustable bracket used in the refining method of the metal beryllium; the method can effectively remove the impurity contents of Li, Pb, Mg, K and Zn in the pure beryllium, and improve the grade of the pure beryllium.
Description
Technical Field
The invention relates to a refining method and a refining device for metallic beryllium, and belongs to the field of metallurgy and materials.
Background
The metal beryllium is relatively active, the melting point of the metal beryllium is that an oxide film is easily formed on the surface of the metal beryllium exposed in the air for passivation, the film is hard and compact in texture and high in melting point, the beryllium can be protected from being continuously oxidized, and a hard wrapping layer can be formed at high temperature to prevent internal volatile gas from overflowing. The characteristics bring great influence on the vacuum volatilization impurity removal process, for the alloy with high content of volatile impurities, for example, the content of Mg impurities in 95 wt% Be is more than 3wt%, Mg steam can form huge bubbles to break the package of the beryllium oxide film in vacuum volatilization, a large number of cavities are formed on the surface of the raw material, and a channel is provided for further volatilization of trace Mg; for pure metals with low impurity content, for example, Be-4 has Mg content of less than 1wt%, and the Mg vapor amount in vacuum volatilization is too small, so that a large number of micro bubbles can Be formed, and the beryllium oxide film can not Be broken through. Therefore, the conventional batch reaction kettle is adopted to execute the vacuum volatilization impurity removal process, and the impurity removal effect of the raw material with higher purity is not as good as that of the raw material with higher impurity content.
After the metallic beryllium had melted, the density of the beryllium was 1.848g/cm3The beryllium oxide density was 3.025 g/cm3So old beryllium oxide will precipitate to form the bottom coating; the internal environment of the industrial volatilization furnace also contains a small amount of oxygen, and the oxidant brought by the raw material can oxidize the metal beryllium with exposed surfaces to form a new beryllium oxide hard shell, and the new and old hard shells close the upper and lower passages. Refining of metals by conventional vacuum distillationBeryllium can only be removed by a method of multiple distillation, such as secondary distillation and tertiary distillation … …, so that the process is complicated and the effect is not good.
Disclosure of Invention
In order to break through the wrapping of a surface beryllium oxide film, a refining method of metal beryllium comprises the steps of heating beryllium beads containing impurities in an oxygen-free environment, wherein the heating temperature is higher than the melting point of beryllium and the boiling point of the impurities, when the boiling point of the impurities is higher than the melting point of beryllium, the beryllium is melted firstly, and is continuously heated to be higher than the boiling point of the impurities, the beryllium beads are melted to form liquid drops, the liquid drops emerge from a side hole of a raw material crucible at a high position and drop down, and in the dropping process, the impurities are volatilized to obtain refined beryllium; when the boiling point of the impurities is lower than the melting point of beryllium, the impurities are volatilized firstly, but the volatilization amount is small, the impurities are continuously heated to be higher than the melting point of the beryllium, liquid drops are formed after beryllium beads are melted, the liquid drops emerge from side holes of a crucible for raw materials at a high position and drop down, and the impurities are volatilized in the dropping process to obtain refined beryllium; and refining the beryllium by further volatilization in a liquid state.
After the impurity content, the size of the liquid drop, the temperature and the pressure are fixed, the volatilization speed of the impurity is a fixed value, in order to improve the total volatilization amount of the impurity in the falling process, the volatilization time can be prolonged, the falling distance of the metal liquid drop is changed by adjusting the distance d between the raw material crucible and the residue crucible, the dropping time, namely the volatilization time of the impurity is changed, and the volatilization time is prolonged by increasing the distance d between the raw material crucible and the residue crucible for low-grade metal with higher impurity content; the high-grade raw material with low impurity content shortens the volatilization time and improves the production efficiency by shortening the distance d between the raw material crucible and the residue crucible.
The impurities in the beryllium bead containing the impurities are one or more of Zn, Mg, K, Li and Pb.
The oxygen-free environment is that 99.9 percent of the sealed space is inert gas or the vacuum degree is less than 2 mmHg.
The invention also provides a device used in the refining method of the metal beryllium, which comprises an inert gas cylinder 1, a valve 2, a dust removal device 3, a vacuum pump 4, a raw material crucible 6, a support 8, a heating element 10, a shell 11 and a product crucible 15, wherein the dust removal device 3 and the vacuum pump 4 are sequentially arranged at the top of the shell 11, the top of the shell 11 is also connected with the inert gas cylinder 1, the valve 2 is arranged between the inert gas cylinder 1 and the shell 11, the heating element 10 is arranged on the inner wall of the shell 11, the raw material crucible 6, the support 8 and the product crucible 15 are arranged in the shell 11, the raw material crucible 6 is arranged on the support 8, the product crucible 15 is arranged below the raw material crucible 6, more than 1 side hole 12 is formed in the side wall of the raw material crucible 6, and the outer diameter of the bottom of the raw material crucible 6 is smaller than the inner diameter of the top of the product crucible 15.
The support 8 is a telescopic support, the distance between the bottom of the raw material crucible 6 and the bottom of the product crucible 15 is adjusted by adjusting the telescopic length of the support 8, and the rod of the telescopic support is a telescopic rod which is commercially available conventionally.
The heating element 10 is a heating resistor.
The edge of the side hole 12 is 1-60mm away from the bottom of the raw material crucible 6 and is used for storing precipitated beryllium oxide fragments.
Putting beryllium beads containing impurities into a raw material crucible 6, adjusting an expansion link of a support 8 to ensure that the distance between a side hole 12 and the bottom of the crucible meets the requirement, closing a shell 11, closing a valve 2 on a branch of an inert gas cylinder 1, starting a vacuum pump 4, vacuumizing the interior of the shell 11, pumping out air in the shell, and obtaining an oxygen-free environment when the vacuum degree is reduced to below 2 mmHg; or after vacuum pumping, closing the vacuum pump 4, opening the valve 2 on the branch of the inert gas bottle 1, filling the inert gas in the shell 11, wherein the inert gas accounts for more than 99.9 percent and is an oxygen-free environment, starting the heating element 10, heating the interior of the shell 11, when the boiling point of impurities is higher than the melting point of beryllium, melting the beryllium firstly, continuing to heat the beryllium to be higher than the boiling point of the impurities, melting beryllium beads to form liquid drops 14, discharging the liquid drops from the side hole 12 of the high-position raw material crucible 6 and dropping the liquid drops, and volatilizing the impurities in the dropping process to obtain refined beryllium; when the boiling point of the impurities is lower than the melting point of beryllium, the impurities are volatilized firstly, but the volatilization amount is small, the impurities are continuously heated to be higher than the melting point of the beryllium, liquid drops 14 are formed after beryllium beads are melted, the liquid drops emerge from the side holes 12 of the high-position raw material crucible 6 and drop down, and the impurities are volatilized in the dropping process to obtain refined beryllium; and refining the beryllium by further volatilization in a liquid state.
The invention can effectively reduce the impurity content of zinc, magnesium, lead, potassium, lithium and the like in the pure beryllium and improve the grade of the pure beryllium.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
in the figure: 1-inert gas cylinder, 2-valve, 3-dust removal device, 4-vacuum pump, 5-pipeline, 6-raw material crucible, 7-new beryllium oxide crust, 8-support, 9-metallic beryllium melt, 10-heating element, 11-shell, 12-side hole, 13-beryllium oxide fragment, 14-droplet and 15-product crucible.
Detailed Description
Example 1
A refining method of metal beryllium comprises the following steps that raw materials of a certain metal beryllium Be-4 grade of a product Kazakhstan contain 0.4 wt% of trace metal Zn, the mass percentage of the total impurities is 0.95 wt%, the adopted device is shown in figure 1 and comprises an inert gas cylinder 1, a valve 2, a dust removal device 3, a vacuum pump 4, a raw material crucible 6, a support 8, a heating element 10, a shell 11 and a product crucible 15, the top of the shell 11 is sequentially provided with the dust removal device 3 and the vacuum pump 4 through a pipeline 5, the top of the shell 11 is also connected with the inert gas cylinder 1 through a pipeline, the valve 2 is arranged between the inert gas cylinder 1 and the shell 11, inert gas nitrogen is filled in the inert gas cylinder 1, the heating element 10 is arranged on the inner wall of the shell 11, the heating element 10 is a heating resistor, the raw material crucible 6, the support 8 and the product crucible 15 are arranged in the shell 11, the raw material crucible 6 is arranged on a support 8, the support 8 is a telescopic support, the product crucible 15 is arranged below the raw material crucible 6, 2 side holes 12 are formed in the side wall of the raw material crucible 6, the outer diameter of each side hole 12 is 10mm, the outer diameter of the bottom of the raw material crucible 6 is smaller than the inner diameter of the top of the product crucible 15, the outer diameter of the bottom of the raw material crucible 6 is 80mm, the inner diameter of the product crucible 15 is 100mm, the distance "d" from the side hole 12 to the bottom of the raw material crucible 6 is 5mm, the bottom is used for storing precipitated beryllium oxide fragments, and the distance "d" between the bottom of the raw material crucible 6 and the bottom of the product crucible 15 is adjusted to be 130mm by adjusting the telescopic length of the support 8; the specific method comprises the following steps:
placing metal beryllium beads in a raw material crucible 6, adjusting an expansion link of a support 8 to ensure that the distance between a side hole 12 and the bottom of the crucible meets the requirement, closing a shell 11, closing a valve 2 on a branch of an inert gas cylinder 1, starting a vacuum pump 4, vacuumizing the interior of the shell 11, closing the vacuum pump 4, opening the valve 2 on the branch of the inert gas cylinder 1 to ensure that the interior of the shell 11 is filled with inert gas, wherein the inert gas accounts for more than 99.9 percent and is also in an oxygen-free environment, heating the interior of the shell 7 by a heating element 6, the boiling point of zinc impurity under 760mmHg is 907 ℃ and is lower than the melting point 1287 ℃ of beryllium, continuing to rapidly heat to 1307 ℃ and about 20 ℃ higher than the melting point of beryllium to keep the temperature, the average volatilization speed of Zn is 16mg/S, the average falling time is 0.25 seconds, forming metal beryllium 9 after the raw material is melted, breaking through the wrapping of an oxide film at the side hole 12 of the crucible, forming liquid drops 14, dropping from the side holes 8 under the action of gravity, wherein in the dropping process, volatile impurity zinc is quickly gasified to form metal steam, a new oxidation film cannot be formed on the surface of the liquid drops 14 in an oxygen-free environment, zinc in beryllium is smoothly volatilized and separated from the metal liquid drops in the dropping process, most of the metal steam enters the dust removal device 3 along the air exhaust pipeline 5 to finish cooling and dust collection so as to prevent impurities from entering the vacuum pump 2, a small amount of the metal steam is condensed on the inner wall of the shell 11, condensate in the inner wall of the shell 11 and the dust removal device 3 needs to be regularly cleaned, the non-volatilized part falls into the product crucible 15 to obtain refined beryllium, liquid is kept, trace volatile impurities can be further volatilized until the raw material is completely dripped, the mass percentage content of Zn in the refined beryllium in the product crucible 15 is reduced to 0.002 wt%, the mass percentage content of the total amount of the impurities is reduced to 0.15wt%, the requirement of Be-2 energy level is met, beryllium oxide fragments 13 on the surfaces of beryllium balls serving as raw materials are stored at the bottom of the raw material crucible 6, and the beryllium oxide precipitate 13 at the bottom of the crucible 6 with the opening in the side wall can Be cleaned after refining is finished, so that the materials can Be charged again.
The method adopts a common rotary-vane vacuum pump, a fixed-kettle crucible and a vacuum metallurgical furnace, the volatilization vacuum degree is 1mmHg, the heating temperature is 1278 ℃, and after the traditional vacuum volatilization purification, the Zn content of the raw material is reduced to 0.35 wt%, and the total impurity content is reduced to 0.89 wt%.
Example 2
A method for refining metallic beryllium, a certain metallic beryllium which is produced by the water outlet of the south mountain of the lake of China is prepared by Mg thermal reduction, the raw material contains a large amount of metallic magnesium (the mass percentage content is about 2-5 wt%) and contains a trace amount of lead, the same device as that of the embodiment 1 is adopted, the number of side holes 12 is 3, the outer diameter of a raw material crucible 6 is 50mm, the inner diameter of a product crucible 15 is 70mm, the distance between the side holes 12 and the raw material crucible 6 'h' is 1mm, different from the embodiment 1, because the total amount of the impurities is larger, the length of an adjustable bracket 8 needs to be increased to 200mm, the distance'd' between the bottom of the side wall opening crucible 6 and the bottom of the product crucible 15 is 150mm, and the volatilization time of liquid drops is increased by increasing the falling distance of the metallic liquid drops, the specific method is as follows:
placing metal beryllium beads in a raw material crucible 6, adjusting an expansion link of a support 8 to enable the distance between a side hole 12 and the bottom of the crucible to meet the requirement, closing a shell 11, closing a valve 2 on a branch of an inert gas cylinder 1, starting a vacuum pump 4, vacuumizing the interior of the shell 11, pumping out air in the shell, and reducing the vacuum degree to 1mmHg to obtain an oxygen-free environment, wherein trace oxygen elements oxidize beryllium on the surface layer to form a new beryllium oxide hard shell 7. At this time, the boiling point of Mg is 605 ℃, the boiling point of lead is 977 ℃ and is lower than the melting point of beryllium 1287 ℃, the heating element 10 is started, the heating temperature is 1327 ℃ and is about 50 ℃ higher than the melting point of beryllium, the average volatilization speed of impurities is 30Mg/S, and the falling time is 0.35 seconds on average. After the metal beryllium is heated to the melting point, the volatilization temperature of the melting point plus 50 ℃ is kept, the raw material is melted to form a metal beryllium melt 9, the package of an oxidation film at the side hole 12 of the crucible is broken through, a liquid drop 14 is formed and drops from the side hole 8 under the action of gravity, in the dropping process, volatile impurity zinc is quickly gasified to form metal steam, no new oxidation film is formed on the surface of the liquid drop 14 in an oxygen-free environment, the zinc in the beryllium is smoothly volatilized and separated from the metal liquid drop in the dropping process, most of the metal steam enters the dust removal device 3 along the air extraction pipeline 5 to finish cooling and dust collection so as to prevent the impurities from entering the vacuum pump 2 and being slightly condensed on the inner wall of the shell 11, condensate in the inner wall of the shell 11 and the dust removal device 3 needs to be periodically cleaned, the non-volatilized part falls into the product crucible 15 to be refined, and the liquid is kept, wherein trace volatile impurities can be further volatilized, until the dripping of the raw materials is finished, trace Mg and Pb in the beryllium are volatilized to Be separated from metal droplets in the dripping process and can Be slowly volatilized after entering a residue crucible, the Mg content of the raw materials is reduced to 0.001wt%, the Pb content is lower than 0.001wt%, the total amount of impurities is reduced to 0.3wt%, and the requirement of Be-1 level is met. And after refining, the beryllium oxide precipitate 13 at the bottom of the crucible 6 with the opening on the side wall is cleaned, and then the materials can be charged again.
After the same dropping time as in example 2 was carried out by conventional vacuum evaporation purification, the raw material contained Mg in an amount of 0.95 wt%, Pb in an amount of 0.005 wt%, and the total impurities in an amount of 0.13 wt%, which was Be of a grade of 98.8 wt%.
Example 3
A refining method of metal beryllium is characterized in that certain metal beryllium which is produced from a water outlet of a southern mountain of a lake in China is prepared by Mg thermal reduction, the raw material contains a large amount of metal magnesium (the mass percentage content is about 2-5 wt%), the device which is the same as that in the embodiment is adopted, the number of side holes 12 is 3, the outer diameter of a raw material crucible 6 is 50mm, the inner diameter of a product crucible 15 is 70mm, the 'h' of the side hole 12, which is far away from the crucible 6 with an opening on the side wall, is increased to 60mm, different from the embodiments 1 and 2, beryllium oxide fragments 13 on the surfaces of beryllium balls which are used as the raw material are stored at the bottom of the raw material crucible 6, and the beryllium oxide fragments can be accumulated after the last refining is finished without cleaning the crucible 6 with the opening on the side wall. The specific method comprises the following steps:
placing metal beryllium beads in a raw material crucible 6, adjusting an expansion link of a support 8 to ensure that the distance between a side hole 12 and the bottom of the crucible meets the requirement, closing a shell 11, closing a valve 2 on a branch of an inert gas cylinder 1, starting a vacuum pump 4, vacuumizing the interior of the shell 11, pumping out air in the shell, and reducing the vacuum degree to 1mmHg to obtain an oxygen-free environment, wherein the boiling point of Mg is 605 ℃, the temperature is lower than the melting point 1287 ℃ of beryllium, the heating temperature is 1327 ℃, the temperature is higher than the melting point of beryllium by about 50 ℃, the average volatilization speed of impurities is 30Mg/S, and the falling time is 0.37 seconds on average. After the metal beryllium is heated to the melting point, the volatilization temperature of the melting point plus 50 ℃ is kept, the raw material is melted to form a metal beryllium melt 9, the package of an oxidation film at the side hole 12 of the crucible is broken through, a liquid drop 14 is formed and drops from the side hole 8 under the action of gravity, in the dropping process, volatile impurity zinc is quickly gasified to form metal steam, no new oxidation film is formed on the surface of the liquid drop 14 in an oxygen-free environment, the zinc in the beryllium is smoothly volatilized and separated from the metal liquid drop in the dropping process, most of the metal steam enters the dust removal device 3 along the air extraction pipeline 5 to finish cooling and dust collection so as to prevent the impurities from entering the vacuum pump 2 and being slightly condensed on the inner wall of the shell 11, condensate in the inner wall of the shell 11 and the dust removal device 3 needs to be periodically cleaned, the non-volatilized part falls into the product crucible 15 to be refined, and the liquid is kept, wherein trace volatile impurities can be further volatilized, until the dripping of the raw materials is finished, the trace Mg in the beryllium is volatilized to Be separated from the metal droplets in the dripping process and can Be slowly volatilized after entering a residue crucible, the Mg content of the raw materials is reduced to 0.001wt%, the total amount of impurities is reduced to 0.28wt%, and the Be-1 level requirement is met. The bottom of the raw material crucible 6 holds a large amount of beryllium oxide fragments 13 deposited many times.
After the same dropping time as in example 2, the Mg content of the raw material was reduced to 0.95 wt% and the total impurity content was reduced to 0.13 wt%, which was a grade of Be 98.8 wt%, by conventional vacuum evaporation purification.
Claims (2)
1. A refining method of metal beryllium is characterized in that beryllium balls containing impurities are placed in a raw material crucible (6), the expansion of a support (8) is adjusted to enable the distance between a side hole (12) and the bottom of the crucible to meet requirements, a shell (11) is closed, a valve (2) on a branch of an inert gas cylinder (1) is closed, a vacuum pump (4) is started, the interior of the shell (11) is vacuumized, air in the shell is pumped out, and the oxygen-free environment is obtained when the vacuum degree is reduced to below 2 mcng; or after vacuum pumping, closing the vacuum pump (4), opening a valve (2) on a branch of the inert gas bottle (1), filling inert gas in the shell (11), wherein the inert gas accounts for more than 99.9 percent and is also in an oxygen-free environment, starting the heating element (10), heating the interior of the shell (11), when the boiling point of impurities is higher than the melting point of beryllium, melting beryllium firstly, continuing to heat to be higher than the boiling point of the impurities, forming liquid drops (14) after beryllium beads are melted, overflowing from side holes (12) of the raw material crucible (6) and dropping, and volatilizing the impurities in the dropping process to obtain refined beryllium; when the boiling point of impurities is lower than the melting point of beryllium, the impurities are volatilized firstly, the impurities are continuously heated to be higher than the melting point of the beryllium, liquid drops (14) are formed after beryllium balls are melted, the liquid drops emerge from side holes (12) of a high-position raw material crucible (6) and drop down, a new oxidation film cannot be formed on the surfaces of the liquid drops (14) in an oxygen-free environment, the impurities in the beryllium are volatilized smoothly and separated from metal liquid drops in the dropping process, most of metal steam enters a dust removal device (3) along an air extraction pipeline (5) to finish cooling and dust collection so as to prevent the impurities from entering a vacuum pump (4), a small amount of the metal steam is condensed on the inner wall of a shell (11), condensate in the inner wall of the shell (11) and the dust removal device (3) is cleaned regularly, the non-volatilized part falls into a product crucible (15) to obtain refined beryllium, liquid is kept, and trace volatile impurities are further volatilized until the raw material is completely dropped.
2. The refining method of metallic beryllium according to claim 1, wherein the used devices comprise an inert gas cylinder (1), a valve (2), a dust removal device (3), a vacuum pump (4), a raw material crucible (6), a support (8), a heating element (10), a shell (11) and a product crucible (15), the dust removal device (3) and the vacuum pump (4) are sequentially arranged at the top of the shell (11), the top of the shell (11) is also connected with the inert gas cylinder (1), the valve (2) is arranged between the inert gas cylinder (1) and the shell (11), the heating element (10) is arranged on the inner wall of the shell (11), the raw material crucible (6), the support (8) and the product crucible (15) are arranged in the shell (11), the raw material crucible (6) is arranged on the support (8), the product crucible (15) is arranged below the raw material crucible (6), more than 1 side hole (12) is formed in the side wall of the raw material crucible (6), the outer diameter of the bottom of the raw material crucible (6) is smaller than the inner diameter of the top of the product crucible (15).
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