Preparation process of high-purity micron-sized metal beryllium powder

Abstract

The invention relates to the technical field of metal beryllium powder, in particular to a preparation process of high-purity micron-sized metal beryllium powder, which comprises the following steps: (1) obtaining beryllium hydroxide; (2) obtaining basic beryllium acetate; (3) obtaining high-purity basic beryllium acetate; (4) obtaining high-purity beryllium oxide; (5) forming a molten salt system; (6) adding high-purity beryllium oxide into the molten salt system, uniformly mixing, and electrolyzing under the protection of inert atmosphere to obtain high-purity micron-sized metal beryllium powder; according to the method, the high-purity metal beryllium powder with the particle size as low as micron can be obtained, is small in particle size and uniform in distribution, has high thermal conductivity and good electromagnetic performance, and can be used for manufacturing electronic elements and magnetic recording materials; the magnetic recording material prepared from the high-purity micron-sized metal beryllium powder has the advantages of high stability, clear image, high signal-to-noise ratio, small distortion and the like.

Description

Technical Field

[0001] The invention relates to the technical field of metal beryllium powder, in particular to a preparation process of high-purity micron-grade metal beryllium powder. Background Art

[0002] The density of metallic beryllium is comparable to that of metallic magnesium, and its stiffness is similar to that of metallic tungsten. The melting point of metallic beryllium is as high as 1278°C, and it has very strong thermal neutron scattering capability. When the temperature changes by hundreds of degrees Celsius, metallic beryllium can maintain its original size, and its performance stability is relatively high.

[0003] The excellent properties of metallic beryllium enable it to be used in a variety of high-end fields, including military industry, aerospace, etc.

[0004] However, the purity of beryllium powder prepared by the existing technology is relatively low, usually only reaching about 86-98%, while high-purity beryllium powder has a wider range of applications. Therefore, it is necessary to further improve the existing technology to improve the application performance of metal beryllium powder. Summary of the invention

[0005] In view of the problems existing in the prior art, the present invention provides a preparation process of high-purity micron-grade metal beryllium powder.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A preparation process of high-purity micron-grade metal beryllium powder comprises the following steps:

[0008] (1) Adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 2-3 hours, and filtering to obtain beryllium hydroxide;

[0009] (2) mixing the obtained beryllium hydroxide with glacial acetic acid for reaction, and after the reaction is completed, diluting with water, letting it stand and then filtering to obtain basic beryllium acetate;

[0010] (3) heating and subliming the basic beryllium acetate to obtain high-purity basic beryllium acetate;

[0011] (4) placing high-purity basic beryllium acetate in a vacuum furnace for heating, keeping the temperature, and cooling to room temperature to obtain high-purity beryllium oxide;

[0012] (5) mixing ammonium fluoroberyllate, chloride salt and fluoride salt uniformly and placing them in a crucible to melt to form a molten salt system;

[0013] (6) High-purity beryllium oxide is added to the molten salt system, mixed evenly, and then electrolyzed under the protection of an inert atmosphere to obtain high-purity micron-sized metallic beryllium powder.

[0014] As a further technical solution, in step (1), the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 12-15 g:100 g;

[0015] The mass fraction of the sodium hydroxide solution is 50-60%;

[0016] The amount of pure water added is 20-40 times the mass of industrial-grade beryllium oxide;

[0017] The heating temperature of the heating and stirring is 85-88°C, and the stirring speed is 550r / min.

[0018] As a further technical solution, in step (2),

[0019] The mixed reaction comprises: pre-heating glacial acetic acid at a temperature of 50-60° C. for 30 minutes; adding beryllium hydroxide to the pre-heated glacial acetic acid, continuing to heat and stir for 15-18 hours, then diluting with water, standing, filtering, washing, and drying to obtain basic beryllium acetate;

[0020] Wherein, adding water to dilute means adding 15-20 times the mass of pure water to the reaction system for dilution;

[0021] The resting time is 4 hours;

[0022] Washing means washing with pure water until neutral;

[0023] Drying refers to drying at 60°C for 4 hours.

[0024] As a further technical solution, the molar ratio of beryllium hydroxide and glacial acetic acid in step (2) is 1:2.

[0025] As a further technical solution, the heating sublimation temperature in step (3) is 260-300°C.

[0026] As a further technical solution, in step (4), the heating temperature of the vacuum furnace is 650-800° C. and the temperature is kept at 4-8 hours.

[0027] As a further technical solution, in step (5), the molar ratio of ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:1.

[0028] As a further technical solution, the chloride salt in step (5) is potassium chloride;

[0029] The fluoride salt is potassium fluoride.

[0030] As a further technical solution, in step (6), high-purity beryllium oxide is added to the molten salt system:

[0031] Under stirring conditions, high-purity beryllium oxide is added into the molten salt system;

[0032] The addition amount of high-purity beryllium oxide is 30-35% of the mass of the molten salt system.

[0033] As a further technical solution, the inert atmosphere in step (6) is a neon atmosphere;

[0034] The electrolysis parameters are:

[0035] The electrolysis temperature is 650°C and the current density during the electrolysis process is 0.8-1.2A / cm 2 , the electrolysis electrode distance is 12-15cm, and the electrolysis time is 10-12 hours;

[0036] The electrolytic electrode in step (6) is:

[0037] Anode carbon rod, cathode chromium rod.

[0038] Compared with the prior art, the present invention has the following beneficial effects:

[0039] The method of the present invention can obtain metal beryllium powder with a particle size as low as micron level, has high thermal conductivity and good electromagnetic properties, and can be used to manufacture electronic components, including integrated circuit boards, transistors, etc.

[0040] The high-purity micron-grade metal beryllium powder prepared by the present invention can be used to prepare magnetic recording materials due to its unique properties. The magnetic recording materials prepared by the present invention have the advantages of high stability, clear image, high signal-to-noise ratio and low distortion, and have a wide range of applications.

[0041] Since the metal beryllium powder prepared by the present invention has a small particle size and uniform distribution, a high specific surface area, a high filling density and high temperature resistance, it can be used to manufacture high-temperature fuel components and engine components that withstand high temperatures, and can greatly improve the safety and reliability of the components.

[0042] On the basis of the existing technical solutions, the method of the present invention can further obtain beryllium oxide with higher purity by preliminary treatment of industrial-grade beryllium oxide, thereby paving the way for obtaining metal beryllium powder with higher purity. After electrolytic treatment, metal beryllium powder with higher purity can be obtained. The purity of the metal beryllium powder prepared by the present invention can reach 4N.

[0043] When preparing metallic beryllium powder by electrolysis, the kinetics of the electrode reaction plays a key role in the deposition process of metallic beryllium. On the cathode, beryllium ions receive electrons and are reduced to metallic beryllium. By controlling the electrolysis conditions, such as current density, electrolyte composition and temperature, the reduction process of beryllium ions on the cathode surface can be made relatively stable and uniform.

[0044] For example, a suitable current density can ensure that beryllium ions are deposited at a relatively uniform rate on the cathode. If the current density is too high, it may cause the local potential to be too high, causing beryllium ions to deposit quickly at certain active sites, forming uneven particles; while at a suitable current density, beryllium ions uniformly obtain electrons on the cathode surface and deposit, which is conducive to the generation of beryllium powder with uniform particle size.

[0045] During the electrolysis process, the standard electrode potential of beryllium is low. Under a certain electrolysis potential, beryllium ions are preferentially deposited at the cathode, thereby reducing the inclusion of impurity metals in the beryllium powder and improving the purity of the beryllium powder.

[0046] Compared with the traditional preparation method, the production cycle of the high-purity micron-level metal beryllium powder prepared by the present invention is shorter, a large amount of high-purity micron-level metal beryllium powder can be obtained in a shorter time, and the process of the present invention does not cause pollution to the environment.

[0047] The micron-grade beryllium powder prepared by the present invention has multiple advantages and characteristics such as high purity, strong process controllability, high production efficiency and environmental protection, and has broader application prospects and development potential. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.

[0049] Figure 1 This is a statistical chart of the particle size of metal beryllium powder in each group of experiments. DETAILED DESCRIPTION

[0050] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0051] The following are specific embodiments:

[0052] Example 1

[0053] A preparation process of high-purity micron-grade metal beryllium powder comprises the following steps:

[0054] (1) Adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 2 hours, and filtering to obtain beryllium hydroxide; the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 12g:100g; the mass fraction of the sodium hydroxide solution is 50%; the amount of pure water added is 20 times the mass of the industrial-grade beryllium oxide; the heating temperature of the heating and stirring is 85°C, and the stirring speed is 550r / min.

[0055] (2) The obtained beryllium hydroxide is mixed with glacial acetic acid for reaction. After the reaction is completed, water is added to dilute it, and it is allowed to stand for 4 hours before filtering to obtain basic beryllium acetate. The mixed reaction is as follows: the glacial acetic acid is pre-insulated at a temperature of 50° C. for 30 minutes; the beryllium hydroxide is added to the pre-insulated glacial acetic acid, and the reaction is continued for 15 hours after being heated and stirred, and then diluted with water, allowed to stand, filtered, washed, and dried to obtain basic beryllium acetate. Among them, diluting with water means adding 15 times the mass of pure water to the reaction system for dilution; the standing time is 4 hours; washing means washing with pure water until neutral; drying means drying at a temperature of 60° C. for 4 hours; the molar ratio of the beryllium hydroxide to the glacial acetic acid is 1:2.

[0056] (3) Subliming the basic beryllium acetate by heating to obtain high-purity basic beryllium acetate; the sublimation temperature is 260°C.

[0057] (4) High-purity basic beryllium acetate is placed in a vacuum furnace for heating, heat preservation, and cooling to room temperature to obtain high-purity beryllium oxide; the vacuum furnace is heated to 650° C. and heat preservation is performed for 4 hours.

[0058] (5) The ammonium fluoroberyllate, chloride salt and fluoride salt are mixed evenly and then placed in a crucible to melt to form a molten salt system; the molar ratio of the ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:1. The chloride salt is potassium chloride; and the fluoride salt is potassium fluoride.

[0059] (6) adding high-purity beryllium oxide to the molten salt system, mixing evenly, and then electrolyzing under the protection of an inert atmosphere to obtain high-purity micron-grade metallic beryllium powder; adding high-purity beryllium oxide to the molten salt system comprises: adding high-purity beryllium oxide to the molten salt system under stirring conditions; wherein the amount of high-purity beryllium oxide added is 30% of the mass of the molten salt system; the inert atmosphere is a neon atmosphere; wherein the electrolysis parameters are: the electrolysis temperature is 650° C., and the current density during the electrolysis process is 0.8 A / cm 2 The electrolysis electrode distance is 12 cm and the electrolysis time is 10 hours; the electrolysis electrodes are: anode carbon rod and cathode chromium rod.

[0060] Example 2

[0061] A preparation process of high-purity micron-grade metal beryllium powder comprises the following steps:

[0062] (1) Adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 2.25 hours, and filtering to obtain beryllium hydroxide; the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 13g:100g; the mass fraction of the sodium hydroxide solution is 52.5%; the amount of pure water added is 25 times the mass of the industrial-grade beryllium oxide; the heating temperature of the heating and stirring is 86°C, and the stirring speed is 550r / min.

[0063] (2) The obtained beryllium hydroxide is mixed with glacial acetic acid for reaction. After the reaction is completed, water is added to dilute it, and it is allowed to stand for 4 hours before filtering to obtain basic beryllium acetate. The mixed reaction is as follows: the glacial acetic acid is pre-insulated at a temperature of 52.5°C for 30 minutes; the beryllium hydroxide is added to the pre-insulated glacial acetic acid, and the reaction is continued for 15.75 hours after being heated and stirred, and then diluted with water, allowed to stand, filtered, washed, and dried to obtain basic beryllium acetate; wherein, diluting with water refers to adding 16.25 times the mass of pure water to the reaction system for dilution; the standing time is 4 hours; washing refers to washing with pure water until neutral; drying refers to drying at a temperature of 60°C for 4 hours; the molar ratio of the beryllium hydroxide to the glacial acetic acid is 1:2.

[0064] (3) Subliming the basic beryllium acetate by heating to obtain high-purity basic beryllium acetate; the sublimation temperature is 275°C.

[0065] (4) High-purity basic beryllium acetate is placed in a vacuum furnace for heating, heat preservation, and cooling to room temperature to obtain high-purity beryllium oxide; the vacuum furnace is heated to 700° C. and heat preservation is performed for 5 hours.

[0066] (5) The ammonium fluoroberyllate, chloride salt and fluoride salt are mixed evenly and then placed in a crucible to melt to form a molten salt system; the molar ratio of the ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:1. The chloride salt is potassium chloride; and the fluoride salt is potassium fluoride.

[0067] (6) adding high-purity beryllium oxide to the molten salt system, mixing evenly, and electrolyzing under the protection of an inert atmosphere to obtain high-purity micron-grade metallic beryllium powder; adding high-purity beryllium oxide to the molten salt system comprises: adding high-purity beryllium oxide to the molten salt system under stirring conditions; wherein the amount of high-purity beryllium oxide added is 31.25% of the mass of the molten salt system; the inert atmosphere is a neon atmosphere; wherein the electrolysis parameters are: the electrolysis temperature is 650° C., and the current density during the electrolysis process is 0.9 A / cm 2 The electrolysis electrode distance is 13 cm and the electrolysis time is 10.5 hours. The electrolysis electrodes are: anode carbon rod and cathode chromium rod.

[0068] Example 3

[0069] A preparation process of high-purity micron-grade metal beryllium powder comprises the following steps:

[0070] (1) Adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 2.75 hours, and filtering to obtain beryllium hydroxide; the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 14g:100g; the mass fraction of the sodium hydroxide solution is 57.5%; the amount of pure water added is 35 times the mass of the industrial-grade beryllium oxide; the heating temperature of the heating and stirring is 87°C, and the stirring speed is 550r / min.

[0071] (2) The obtained beryllium hydroxide is mixed with glacial acetic acid for reaction. After the reaction is completed, water is added to dilute it, and it is allowed to stand for 4 hours before filtering to obtain basic beryllium acetate. The mixed reaction is as follows: the glacial acetic acid is pre-insulated at a temperature of 57.5°C for 30 minutes; the beryllium hydroxide is added to the pre-insulated glacial acetic acid, and the reaction is continued for 17.25 hours after being heated and stirred, and then diluted with water, allowed to stand, filtered, washed, and dried to obtain basic beryllium acetate; wherein, diluting with water refers to adding 18.75 times the mass of pure water to the reaction system for dilution; the standing time is 4 hours; washing refers to washing with pure water until neutral; drying refers to drying at a temperature of 60°C for 4 hours; the molar ratio of the beryllium hydroxide to the glacial acetic acid is 1:2.

[0072] (3) Subliming the basic beryllium acetate by heating to obtain high-purity basic beryllium acetate; the sublimation temperature is 285°C.

[0073] (4) High-purity basic beryllium acetate is placed in a vacuum furnace for heating, heat preservation, and cooling to room temperature to obtain high-purity beryllium oxide; the vacuum furnace is heated to 750° C. and heat preservation is performed for 7 hours.

[0074] (5) The ammonium fluoroberyllate, chloride salt and fluoride salt are mixed evenly and then placed in a crucible to melt to form a molten salt system; the molar ratio of the ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:1. The chloride salt is potassium chloride; and the fluoride salt is potassium fluoride.

[0075] (6) adding high-purity beryllium oxide to the molten salt system, mixing evenly, and then electrolyzing under the protection of an inert atmosphere to obtain high-purity micron-grade metallic beryllium powder; adding high-purity beryllium oxide to the molten salt system comprises: adding high-purity beryllium oxide to the molten salt system under stirring conditions; wherein the amount of high-purity beryllium oxide added is 33.75% of the mass of the molten salt system; the inert atmosphere is a neon atmosphere; wherein the electrolysis parameters are: the electrolysis temperature is 650° C., and the current density during the electrolysis process is 1.1 A / cm 2 The electrolysis electrode distance is 14 cm and the electrolysis time is 11.5 hours. The electrolysis electrodes are: anode carbon rod and cathode chromium rod.

[0076] Example 4

[0077] A preparation process of high-purity micron-grade metal beryllium powder comprises the following steps:

[0078] (1) Adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 3 hours, and filtering to obtain beryllium hydroxide; the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 15g:100g; the mass fraction of the sodium hydroxide solution is 60%; the amount of pure water added is 40 times the mass of the industrial-grade beryllium oxide; the heating temperature of the heating and stirring is 88°C, and the stirring speed is 550r / min.

[0079] (2) The obtained beryllium hydroxide is mixed with glacial acetic acid for reaction. After the reaction is completed, water is added to dilute it, and it is allowed to stand for 4 hours before filtering to obtain basic beryllium acetate. The mixed reaction is as follows: the glacial acetic acid is pre-insulated at a temperature of 60° C. for 30 minutes; the beryllium hydroxide is added to the pre-insulated glacial acetic acid, and the reaction is continued for 18 hours after being heated and stirred, and then diluted with water, allowed to stand, filtered, washed, and dried to obtain basic beryllium acetate. Among them, diluting with water means adding 20 times the mass of pure water to the reaction system for dilution; the standing time is 4 hours; washing means washing with pure water until neutral; drying means drying at a temperature of 60° C. for 4 hours; the molar ratio of the beryllium hydroxide to the glacial acetic acid is 1:2.

[0080] (3) Subliming the basic beryllium acetate by heating to obtain high-purity basic beryllium acetate; the sublimation temperature is 300°C.

[0081] (4) High-purity basic beryllium acetate is placed in a vacuum furnace for heating, heat preservation, and cooling to room temperature to obtain high-purity beryllium oxide; the vacuum furnace is heated to 800° C. and heat preservation is performed for 8 hours.

[0082] (5) The ammonium fluoroberyllate, chloride salt and fluoride salt are mixed evenly and then placed in a crucible to melt to form a molten salt system; the molar ratio of the ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:1. The chloride salt is potassium chloride; and the fluoride salt is potassium fluoride.

[0083] (6) adding high-purity beryllium oxide to the molten salt system, mixing evenly, and then electrolyzing under the protection of an inert atmosphere to obtain high-purity micron-grade metallic beryllium powder; adding high-purity beryllium oxide to the molten salt system comprises: adding high-purity beryllium oxide to the molten salt system under stirring conditions; wherein the amount of high-purity beryllium oxide added is 35% of the mass of the molten salt system; the inert atmosphere is a neon atmosphere; wherein the electrolysis parameters are: the electrolysis temperature is 650° C., and the current density during the electrolysis process is 1.2 A / cm 2 The electrolysis electrode distance is 15 cm and the electrolysis time is 12 hours; the electrolysis electrodes are: anode carbon rod and cathode chromium rod.

[0084] Comparative Example 1: This comparative example is substantially the same as Example 1, except that the high-purity beryllium oxide added to the molten salt system is replaced by industrial-grade beryllium oxide (98%).

[0085] test:

[0086] The purity of the samples of the embodiment and the comparative example was tested by inductively coupled plasma mass spectrometry, and the results are shown in Table 1 below:

[0087] Table 1

[0088] purity% Example 1 99.9893 Example 2 99.9904 Example 3 99.9897 Example 4 99.9914 Comparative Example 1 99.9786

[0089] It can be seen from Table 1 that the metal beryllium powder obtained by the preparation method of the present invention has a higher purity.

[0090] The particle size of the samples of the embodiment and the comparative example was tested according to GB / T1480-2012. The results are shown in Table 2 below:

[0091] Table 2

[0092] Average particle size μm Example 1 7.83 Example 2 8.22 Example 3 7.69 Example 4 8.43 Comparative Example 1 8.95

[0093] It can be seen from Table 2 that the metal beryllium powder prepared by the method of the present invention has a smaller particle size.

[0094] Based on Example 1, the effects of different electrolysis temperatures on the particle size of metal beryllium powder were compared, and the results are shown in Table 3 below:

[0095] Table 3

[0096] Electrolysis temperature℃ Metal Beryllium Powder Particle Size μm 630 8.28 635 8.16 640 8.10 645 7.96 650 7.83 655 7.94 660 8.11 665 8.09 670 8.14 680 8.22

[0097] It can be seen from Table 3 that with the increase of electrolysis temperature, the particle size of metal beryllium powder first decreases and then increases.

[0098] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A process for preparing high-purity micron-grade metal beryllium powder, characterized in that: The following steps are involved: (1) adding industrial-grade beryllium oxide (98%) to a sodium hydroxide solution, heating and stirring for 20 minutes, then adding pure water, continuing to stir and react for 2-3 hours, and filtering to obtain beryllium hydroxide; (2) mixing the obtained beryllium hydroxide with glacial acetic acid for reaction, and after the reaction is completed, diluting with water, letting it stand and then filtering to obtain basic beryllium acetate; (3) heating and subliming the basic beryllium acetate to obtain high-purity basic beryllium acetate; (4) placing high-purity basic beryllium acetate in a vacuum furnace for heating, keeping the temperature, and cooling to room temperature to obtain high-purity beryllium oxide; (5) mixing ammonium fluoroberyllate, chloride salt and fluoride salt uniformly and placing them in a crucible to melt to form a molten salt system; (6) High-purity beryllium oxide is added to the molten salt system, mixed evenly, and then electrolyzed under the protection of an inert atmosphere to obtain high-purity micron-sized metallic beryllium powder.

2. The process for preparing high-purity micron-grade metal beryllium powder according to claim 1, characterized in that: In step (1), the mixing ratio of industrial-grade beryllium oxide and sodium hydroxide solution is 12-15 g: 100 g; The mass fraction of the sodium hydroxide solution is 50-60%; The amount of pure water added is 20-40 times the mass of industrial-grade beryllium oxide; The heating temperature of the heating and stirring is 85-88°C, and the stirring speed is 550r / min.

3. The process for preparing high-purity micron-grade metal beryllium powder according to claim 1, characterized in that: In step (2), The mixed reaction comprises: pre-heating glacial acetic acid at a temperature of 50-60° C. for 30 minutes; adding beryllium hydroxide to the pre-heated glacial acetic acid, continuing to heat and stir for 15-18 hours, then diluting with water, standing, filtering, washing, and drying to obtain basic beryllium acetate; Wherein, adding water to dilute means adding 15-20 times the mass of pure water to the reaction system for dilution; The resting time is 4 hours; Washing means washing with pure water until neutral; Drying refers to drying at 60°C for 4 hours.

4. The process for preparing high-purity micron-sized metal beryllium powder according to claim 3, characterized in that: The molar ratio of beryllium hydroxide to glacial acetic acid in step (2) is 1:

2.

5. The process for preparing high-purity micron-grade metal beryllium powder according to claim 1, characterized in that: The heating sublimation temperature in step (3) is 260-300°C.

6. The process for preparing high-purity micron-grade metal beryllium powder according to claim 1, characterized in that: In step (4), the vacuum furnace is heated to a temperature of 650-800° C. and kept warm for 4-8 hours.

7. The process for preparing high-purity micron-grade metal beryllium powder according to claim 1, characterized in that: In step (5), the molar ratio of ammonium fluoroberyllate, chloride salt and fluoride salt is 1:1:

1.

8. The process for preparing high-purity micron-sized metal beryllium powder according to claim 7, characterized in that: The chloride salt in step (5) is potassium chloride; The fluoride salt is potassium fluoride.

9. The process for preparing high-purity micron-sized metal beryllium powder according to claim 1, characterized in that: In step (6), high-purity beryllium oxide is added to the molten salt system as follows: Under stirring conditions, high-purity beryllium oxide is added into the molten salt system; The addition amount of high-purity beryllium oxide is 30-35% of the mass of the molten salt system.

10. The process for preparing high-purity micron-sized metal beryllium powder according to claim 1, characterized in that: The inert atmosphere in step (6) is a neon atmosphere; The electrolysis parameters are: The electrolysis temperature is 650°C and the current density during the electrolysis process is 0.8-1.2A / cm 2 , the electrolysis electrode distance is 12-15cm, and the electrolysis time is 10-12 hours; The electrolytic electrode in step (6) is: Anode carbon rod, cathode chromium rod.

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