CN116855770A - Method for preparing 4N 5-grade beryllium ingot from beryllium fluoride - Google Patents
Method for preparing 4N 5-grade beryllium ingot from beryllium fluoride Download PDFInfo
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- CN116855770A CN116855770A CN202310904137.9A CN202310904137A CN116855770A CN 116855770 A CN116855770 A CN 116855770A CN 202310904137 A CN202310904137 A CN 202310904137A CN 116855770 A CN116855770 A CN 116855770A
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- beryllium
- fluoride
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- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052790 beryllium Inorganic materials 0.000 title claims abstract description 78
- 229910001633 beryllium fluoride Inorganic materials 0.000 title claims abstract description 54
- JZKFIPKXQBZXMW-UHFFFAOYSA-L beryllium difluoride Chemical compound F[Be]F JZKFIPKXQBZXMW-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 claims abstract description 45
- 239000002184 metal Substances 0.000 claims abstract description 45
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 28
- 239000011777 magnesium Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002893 slag Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005266 casting Methods 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000004857 zone melting Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 description 17
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 10
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 9
- 239000011324 bead Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000006698 induction Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 229910017060 Fe Cr Inorganic materials 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B35/00—Obtaining beryllium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application relates to a method for preparing 4N5 metallic beryllium from beryllium fluoride, belongs to the technical field of metallic beryllium smelting, and solves the bottleneck of large-scale preparation of high-purity metallic beryllium in the prior art. The application provides a method for preparing a 4N 5-level beryllium ingot, which comprises the following steps: proportioning beryllium fluoride powder and magnesium particles according to a certain proportion; carrying out low-temperature magnesium thermal reaction in a closed atmosphere protection; slowly cooling to room temperature along with the furnace; separating slag and metal beryllium powder; low-temperature vacuum smelting of metal beryllium powder; continuously heating to high temperature, and carrying out vacuum smelting; casting into 4N 5-level beryllium ingots. Smelting in the subsequent area can prepare 5N-level metallic beryllium.
Description
Technical Field
The application relates to the technical field of metal beryllium smelting, in particular to a method for preparing a 4N 5-grade or more metal beryllium ingot.
Background
Beryllium is one of the lightest known metallic structural materials and has the characteristics of high strength, high elastic modulus, low density and the like. Beryllium also has good thermal shock resistance and thermal diffusivity and a very small coefficient of thermal expansion. Beryllium is one of the indispensable materials of nuclear power plants and is also an important aerospace material.
The metal beryllium is an important strategic resource, and the preparation of the metal beryllium requires the magnesium reduction of the beryllium fluoride to obtain beryllium beads, and then refining to obtain various grades of metal beryllium.
The reduction of the metal beryllium beads adopts an intermediate frequency furnace normal pressure magnesia reduction process. The residual magnesium in the beryllium beads reaches 1 percent, and even though the subsequent vacuum distillation is carried out, 4N-grade high-purity metallic beryllium is difficult to obtain.
We have proposed two methods for preparing metallic beryllium (grant publication No. CN113059154B, CN 113186397B), the purity of beryllium reaching the 2N-3N grade, but also not reaching the 4N grade.
It is therefore urgent and necessary to find a method for preparing high purity metallic beryllium from beryllium fluoride.
Disclosure of Invention
In view of the above analysis, the present application aims to provide a method for preparing 4N5 grade beryllium ingot from beryllium fluoride, which is used for breaking through the bottleneck of scale preparation of high purity beryllium.
The application provides a method for preparing a 4N 5-grade beryllium ingot from beryllium fluoride, which comprises the following steps:
step 1, proportioning beryllium fluoride powder and magnesium particles according to a certain proportion;
step 2, performing low-temperature magnesium thermal reaction in the sealed atmosphere protection;
step 3, slowly cooling to room temperature along with the furnace;
step 4, separating slag and metal beryllium powder;
step 5, low-temperature vacuum smelting of the metal beryllium powder;
step 6, continuously heating to high temperature, and carrying out vacuum smelting;
and 7, casting into a metal beryllium ingot.
Further, the purity of the beryllium fluoride powder and the magnesium particles is more than 4N, and the sum of the mass concentrations of elements such as Al, fe and the like in the beryllium fluoride, which are not easy to volatilize under vacuum, is less than 0.001%.
Further, in the step 1, the mol ratio of beryllium fluoride to magnesium metal is 1.5:1 or more.
Further, the heating furnace in the step 2 is protected by argon, a protective cover is covered on the graphite crucible, the heating temperature is 800-900 ℃, and the heat preservation time is 120-180 min.
Further, in the step 5, the heating temperature is 950-1050 ℃, the time is 60-120 min, and the vacuum degree is 50-200 Pa.
Further, in the step 6, the heating temperature is 1300-1400 ℃, the time is 30-60 min, and the vacuum degree is 0.5-20 Pa.
Further, the purity of the metal beryllium prepared from the beryllium fluoride is more than 4N5 grade and above.
Compared with the existing method for preparing the metallic beryllium by using the beryllium fluoride, the method can be used for preparing the metallic beryllium with more than 4N5 grade on a large scale.
Furthermore, after high-temperature smelting, a zone smelting method is connected, and 5N-level metallic beryllium can be prepared by a smelting method which separates out impurities or changes the distribution of the impurities by utilizing the difference of the solubility of the impurities in the solidification state and the melt of the metal.
In the application, the technical schemes can be mutually combined to realize more preferable combination schemes. Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application. The objectives and other advantages of the application may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the application, like reference numerals being used to refer to like parts throughout the several views.
Fig. 1 is a schematic process diagram of a first embodiment.
Fig. 2 is a process schematic diagram of a second embodiment.
Detailed Description
The application provides a method for preparing a 4N 5-grade beryllium ingot from beryllium fluoride, which comprises the following steps:
step 1, proportioning beryllium fluoride powder and magnesium particles according to a certain proportion;
step 2, performing low-temperature magnesium thermal reaction in the sealed atmosphere protection;
step 3, slowly cooling to room temperature along with the furnace;
step 4, separating slag and metal beryllium powder;
step 5, low-temperature vacuum smelting of the metal beryllium powder;
step 6, continuously heating to high temperature, and carrying out vacuum smelting;
and 7, casting into a metal beryllium ingot.
Specifically, impurities in the metal beryllium come from raw materials, beryllium fluoride and metal magnesium, and the quality of the metal beryllium is reduced by 80% due to the fact that the metal beryllium is prepared from the metal beryllium, so that the requirement on the concentration of the impurities is high.
For magnesian reduction, because the impurity content is low and the magnesium content is high, almost all impurities enter the metal beryllium, and some impurities which are easy to volatilize under vacuum, such as Zn, P, bi and the like, are easy to remove in the subsequent vacuum smelting, but elements which are difficult to volatilize under vacuum, such as Fe, al, B, cr and the like, cannot be removed in the vacuum smelting process. The amount of these elements introduced must be tightly controlled. The research of the application shows that for preparing 4N5 metal beryllium, the purity of the beryllium fluoride powder and magnesium particles is more than 4N, and the sum of the mass concentrations of elements such as Al, fe and the like in the beryllium fluoride which are not easy to volatilize under vacuum is less than 0.001 percent.
Specifically, the method for preparing metallic beryllium (authorized publication No. CN 113186397B) provided by us provides 98% purity beryllium beads through low-temperature reduction and high-temperature smelting, because the solubility of metallic magnesium in beryllium liquid is high (1-2%), even if high vacuum (10 Pa) is adopted, the solubility of magnesium is also at 0.005%, and 4N grade metallic beryllium can be prepared through beryllium bead reduction and vacuum distillation to the utmost extent in consideration of other impurities. To produce higher grades requires special methods such as zone melting.
Specifically, in the preparation method of metallic beryllium (the authority publication number CN 113059154B), beryllium bead powder is obtained through low-temperature reduction, and then impurities such as magnesium and the like are leached out through HF, so that the purity of the beryllium bead can reach 3N.
Specifically, in the normal low-temperature reduction process, liquid beryllium fluoride and magnesium are reacted in the early stage to form solid magnesium fluoride and metal beryllium, and the solid magnesium fluoride and the metal beryllium are mixed together, so that the separation effect is poor. Therefore, the application provides a novel low-temperature reduction method, which is to surplus beryllium fluoride, and the reaction process generates magnesium fluoride and metallic beryllium, and the rest part of liquid beryllium fluoride. The rest of the beryllium fluoride and magnesium fluoride form a liquid phase, and the solid state metallic beryllium finally floats on the BeF under the condition because the density is higher than that of the metallic beryllium 2 -MgF 2 Above the liquid composition. Metallic beryllium can also sinter together. After cooling along with the furnace, the metal beryllium block with high purity can be obtained. In theory, the mol ratio of beryllium fluoride to magnesium metal is 1:1, and according to the research of the application, the mol ratio of beryllium fluoride to magnesium metal is 1.5: more than 1, and the superfluous beryllium fluoride can form liquid-phase slag with magnesium fluoride generated by reaction at 800-900 ℃.
In particular, the low-temperature reaction temperature is not too high, because too high temperature can increase volatilization of beryllium fluoride and magnesium metal, and the reaction temperature is too low, beF 2 -MgF 2 Only partially forming a liquid phase, the remainder being solidThe low-temperature reduction temperature is 800-900 ℃, and the heat preservation time is 120-180 min, so that the low-temperature reduction can be fully performed.
Specifically, at 800-900 ℃, beryllium fluoride and magnesium metal still volatilize partially, and in order to reduce volatilization, the application particularly increases the protective cover, and the protective cover is covered on the graphite crucible, so that the volatilization loss of the beryllium fluoride and the magnesium metal is reduced to the greatest extent.
Specifically, the magnesium metal and the beryllium metal generated by the reaction belong to active metals, and even if a protective cover is added, the magnesium metal and the beryllium metal can be partially oxidized by external air, so that argon is introduced into the device for protection, and the oxidation loss of the active metals is reduced to the greatest extent.
Specifically, a small amount of slag composed of beryllium fluoride and magnesium fluoride may be present in the separated metallic beryllium as the furnace cools. In order to remove them, a small amount of metallic beryllium and magnesium fluoride react in a vacuum induction furnace at 950-1050 ℃ under vacuum to produce beryllium fluoride and magnesium fluoride, and both the beryllium fluoride and the magnesium fluoride are removed in a gaseous state under vacuum. The temperature is not too high at this time, and when the temperature is high, the content of solid solution magnesium in the metal beryllium is increased, and particularly, the solubility of magnesium in the beryllium melt is higher. It is relatively difficult to reduce the magnesium content of metallic beryllium. Researches show that the constant temperature time is 60-120 min, and the vacuum degree is 50-200 Pa, so that the unseparated beryllium fluoride and magnesium fluoride in the metal beryllium can be completely removed.
At the moment, the metal beryllium still contains a small amount of impurities, including volatile elements and nonvolatile elements, the nonvolatile elements are strictly controlled during batching, vacuum evaporation is also needed for the volatile elements, the metal beryllium becomes liquid at 1300-1400 ℃, and the volatile elements in the beryllium liquid can be removed under the conditions of 0.5-20 Pa of vacuum degree and 30-60 min of constant temperature.
The heating furnace used in the application can be an induction heating furnace or a resistance heating furnace, atmosphere protection and vacuumizing, and the equipment belongs to conventional equipment, is easy to purchase and realizes large-scale production.
If the method is followed by a zone melting method, the non-volatile elements can be used for preparing 5N-level metallic beryllium by a smelting method which utilizes the difference of the solubility of impurities in the solidification state and the melt of the metal to separate out the impurities or change the distribution of the impurities.
The following detailed description of preferred embodiments of the application is made in connection with the accompanying drawings, which form a part hereof, and together with the description of the embodiments of the application, are used to illustrate the principles of the application and not to limit the scope of the application.
Example 1
In one embodiment of the application, a method for preparing 4N5 metallic beryllium from beryllium fluoride is disclosed.
The main impurity components of the beryllium fluoride used in the application are shown in table 1, the purity of the metal magnesium particles is 4N, two main smelting devices are provided, one is an atmosphere protection resistance heating furnace, the low-temperature reaction of the beryllium fluoride and the magnesium is completed, the 2 nd smelting device is a vacuum smelting furnace, the low-temperature vacuum smelting and the high-temperature vacuum smelting are completed, and the process flow is shown in figure 1.
TABLE 1 Main impurity components of beryllium fluoride/wt%
| Al | Fe | Cr | P | As | Zn | Pb |
| 0.00055 | 0.0002 | 0.00015 | 0.0025 | 0.001 | 0.001 | 0.0015 |
Step 1, beryllium fluoride powder and magnesium particles are mixed according to a mol ratio of 1.6:1, batching;
step 2, filling a sample into a graphite crucible, covering a protective cover on the crucible, placing the crucible into a heating furnace, introducing argon for protection, and then heating to 850 ℃ and keeping the temperature for 150min;
step 3, slowly cooling to room temperature along with the furnace;
step 4, separating slag and metal beryllium powder;
step 5, vacuum smelting the metal beryllium powder at 1000 ℃, wherein the vacuum degree is 100Pa, and the temperature is kept for 80 minutes;
step 6, continuously heating to 1350 ℃, and raising the vacuum degree to 5Pa, and vacuum smelting for 40min;
and 7, casting into a metal beryllium ingot.
99.996% of metallic beryllium ingots were prepared by the above method.
Example two
In one embodiment of the application, a method for preparing 5N metallic beryllium from beryllium fluoride is disclosed.
The main impurity components of the beryllium fluoride used in the application are shown in table 1, the purity of the metal magnesium particles is 4N, two main smelting devices are provided, one is an atmosphere protection induction heating furnace, the low-temperature reaction of the beryllium fluoride and the magnesium is completed, the 2 nd smelting device is a vacuum smelting furnace, the low-temperature vacuum smelting and the high-temperature vacuum smelting are completed, the 3 rd device is a zone smelting furnace, and the process flow is shown in figure 2.
Step 1, beryllium fluoride powder and magnesium particles are mixed according to a mol ratio of 1.7:1, batching.
And 2, filling the sample into a graphite crucible, covering a protective cover on the crucible, placing the crucible into a heating furnace, introducing argon for protection, and then heating to 820 ℃ for 160min at constant temperature.
And 3, slowly cooling to room temperature along with the furnace.
And 4, separating slag and metal beryllium powder.
And 5, vacuum smelting the metal beryllium powder at 1050 ℃, wherein the vacuum degree is 60Pa, and the temperature is kept for 60min.
And 6, continuously heating to 1380 ℃, and raising the vacuum degree to 2Pa, and carrying out vacuum smelting for 50min.
And 7, casting into a metal beryllium ingot.
And 8, placing the sample into a zone melting furnace for smelting.
The 5N-level metal beryllium ingot is prepared by the method.
The present application is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present application are intended to be included in the scope of the present application.
Claims (7)
1. A method of preparing a 4N5 grade beryllium ingot from beryllium fluoride, comprising:
step 1, proportioning beryllium fluoride powder and magnesium particles according to a certain proportion;
step 2, performing low-temperature magnesium thermal reaction in the sealed atmosphere protection;
step 3, slowly cooling to room temperature along with the furnace;
step 4, separating slag and metal beryllium powder;
step 5, low-temperature vacuum smelting of the metal beryllium powder;
step 6, continuously heating to high temperature, and carrying out vacuum smelting;
and 7, casting into a metal beryllium ingot.
2. The method for preparing 4N 5-grade beryllium ingots from beryllium fluoride according to claim 1, wherein the purity of the beryllium fluoride powder and magnesium particles is more than 4N, and the sum of the mass concentrations of elements such as Al, fe and the like in the beryllium fluoride which are not easy to volatilize under vacuum is less than 0.001%.
3. The method for preparing 4N 5-grade beryllium ingot from beryllium fluoride according to claim 1, wherein the mol ratio of beryllium fluoride to magnesium metal in step 1 is 1.5:1 or more.
4. The method for preparing 4N 5-grade beryllium ingot from beryllium fluoride according to claim 1, wherein the heating furnace in the step 2 is protected by argon, a graphite crucible is covered with a protective cover, and the heating temperature is 800-900 ℃, and the heat preservation time is 120-180 min.
5. The method for preparing 4N 5-grade beryllium ingot from beryllium fluoride according to claim 1, wherein the heating temperature is 950-1050 ℃ for 60-120 min and the vacuum degree is 50-200 Pa in the step 5.
6. The method for preparing 4N 5-grade beryllium ingot from beryllium fluoride according to claim 1, wherein in the step 6, the heating temperature is 1300-1400 ℃, the time is 30-60 min, and the vacuum degree is 0.5-20 Pa.
7. The method for preparing 4N5 grade beryllium ingot from beryllium fluoride according to claim 1, wherein the purity of the metallic beryllium is increased to 5N grade by zone melting after each step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310904137.9A CN116855770A (en) | 2023-07-21 | 2023-07-21 | Method for preparing 4N 5-grade beryllium ingot from beryllium fluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310904137.9A CN116855770A (en) | 2023-07-21 | 2023-07-21 | Method for preparing 4N 5-grade beryllium ingot from beryllium fluoride |
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