CN114603155B - Preparation method of ultra-high purity nano-grade metal beryllium powder - Google Patents
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Abstract
The application relates to a preparation method of ultra-high purity nano-micro level metal beryllium powder. Comprising the following steps: heating and dissolving industrial-grade beryllium oxide in a high-concentration sodium hydroxide solution, adding the solution into pure water to generate high-purity beryllium hydroxide, performing hot filtration to obtain high-purity beryllium hydroxide, and evaporating and concentrating the hydrolysate to recover high-concentration alkali liquor for recycling in the dissolving process of industrial beryllium oxide; heating and reacting high-purity beryllium hydroxide with excessive high-purity sodium hydroxide solution, and thermally filtering the reaction solution through a filter element to obtain high-purity sodium beryllium acid solution; introducing high-purity high-pressure hydrogen into a high-pressure reaction kettle to perform medium-temperature hydrothermal reduction reaction to generate nano-micro metal beryllium powder; the high-pressure hydrogen reduction slurry is quickly led into an online filter, solid-liquid quick separation is realized in high-pressure hydrogen atmosphere, nano-micro metal beryllium powder is obtained, the reduction solution is high-purity sodium hydroxide solution, and the reduction solution is circularly used for preparing high-purity sodium beryllium acid solution; washing, separating and dynamically drying the beryllium powder by multistage pure water to obtain the ultra-high purity nano-micro level metal beryllium powder.
Description
Technical Field
The application relates to a preparation method of ultra-high purity nano-grade metal beryllium powder which is a key raw material of national defense industrial high-end equipment. Belonging to the field of rare metal hydrometallurgy.
Background
Beryllium has excellent nuclear performance, thermal performance and optical performance, is praised as 'new era nuclear metal', has extremely important application in the fields of advanced national defense science and technology and aerospace, and is an important ring of national development of advanced national defense technology and strategic emerging industry and is also an important research object for utilization and storage of national strategic resources. Beryllium is used in the forms of beryllium copper, beryllium aluminum and beryllium nickel alloy, high-purity metal beryllium, beryllium oxide and the like in the departments of machinery, electronics, petroleum, chemical industry, traffic, national defense industry and the like. The metal beryllium, especially the ultrapure beryllium, has small density, high strength and excellent nuclear performance, and is widely used as structural materials of missiles and satellites and inertial navigation systems, and is also structural materials of nuclear reactors and nuclear weapons and neutron source materials.
Compared with the traditional magnesian reduction method, the method for purifying the raw materials by high-pressure hydrogen reduction coupling sub-molten salt alkaline hydrolysis has the outstanding advantages that new metal impurities are not introduced in the process, and source impurity reduction is achieved, so that the purity of the metal beryllium is obviously higher than that of the metal beryllium prepared by the magnesian reduction method, the purity of the metal beryllium can be at least 99.99%, and compared with the magnesian reduction method, only beryllium beads can be obtained, and the method can directly obtain nano-grade beryllium powder with more excellent physical properties.
Disclosure of Invention
The application aims to provide a preparation method of ultra-high purity nano-micro level metal beryllium powder which is a key raw material of national defense industry high-end equipment.
In order to achieve the above purpose, the present application adopts the following technical scheme:
a method for preparing ultra-high purity nano-grade metal beryllium powder, which comprises the following steps:
a. purifying beryllium oxide: heating and dissolving industrial-grade beryllium oxide in a high-concentration sodium hydroxide solution, adding the solution into pure water at a certain temperature to perform hydrolysis reaction to generate high-purity beryllium hydroxide, performing hot filtration to obtain high-purity beryllium hydroxide, evaporating and concentrating the hydrolysate to recover high-concentration alkali liquor, and recycling the hydrolysate for the dissolving process of industrial beryllium oxide;
b. preparing a high-purity sodium beryllium acid solution: heating and reacting high-purity beryllium hydroxide with excessive high-purity sodium hydroxide solution, and thermally filtering the reaction solution through a high-precision filter element to obtain high-purity sodium beryllium acid solution;
c. high pressure hydrogen reduction: introducing high-purity high-pressure hydrogen into a high-pressure reaction kettle made of special alloy materials to perform medium-temperature hydrothermal reduction reaction to generate nano-grade metal beryllium powder;
d. and (3) online separation: under the condition that the high-pressure hydrogen reduction slurry is kept in a reaction working condition, under the action of high-pressure pneumatic, the high-pressure hydrogen reduction slurry is quickly led into an online filter, solid-liquid quick separation is realized in a high-pressure hydrogen atmosphere, nano-micro metal beryllium powder is obtained, and the reduction solution is a high-purity sodium hydroxide solution and is circularly used for preparing the high-purity sodium beryllium acid solution;
e. purifying beryllium powder: washing, separating and dynamically drying the beryllium powder by multistage pure water to obtain the ultra-high purity nano-micro level metal beryllium powder.
Based on the preparation method of the ultra-high purity nano-micro grade metal beryllium powder, in the step a, the industrial grade beryllium oxide refers to the beryllium oxide with the purity lower than 99 percent, the beryllium oxide dissolution temperature is 80-150 ℃, the concentration of sodium hydroxide solution is 35-85%, the molar ratio of the beryllium oxide to the sodium hydroxide is 1:2.05-1:2.50, the hydrolysis reaction temperature is 30-90 ℃, and the mass ratio of the beryllium oxide to the pure water is 1:15-1:50; preferably, the dissolution temperature of the beryllium oxide is 100-130 ℃, the concentration of the sodium hydroxide solution is 45-70%, the molar ratio of the beryllium oxide to the sodium hydroxide is 1:2.10-1:2.30, the hydrolysis reaction temperature is 50-80 ℃, and the mass ratio of the beryllium oxide to the pure water is 1:25-1:40.
Based on the preparation method of the ultra-high purity nano-micro grade metal beryllium powder, in the step b, the reaction temperature is 30-80 ℃, the mol ratio of beryllium hydroxide to sodium hydroxide is 1:2.02-1:2.20, the concentration of sodium hydroxide solution is 10-30%, further, the reaction temperature is 40-60 ℃, the mol ratio of beryllium hydroxide to sodium hydroxide is 1:2.05-1:2.10, and the concentration of sodium hydroxide solution is 10-20%.
Further, in the step c, the hydrogen reduction temperature is 200-350 ℃, the reaction time is 2-10 h, and the hydrogen pressure is 50-200 Kg/cm 2 Further, the hydrogen reduction temperature is 250-320 ℃, the reaction time is 3-7 h, and the hydrogen pressure is 100-160 Kg/cm 2 。
Further, in the step d, the online separation temperature is 200-300 ℃, and the hydrogen pressure is 100-160 Kg/cm 2 More preferably, the in-line separation temperature is 240-280 ℃ and the hydrogen pressure is 120-150 Kg/cm 2 。
Further, in the step e, the washing temperature of the metal beryllium powder is 25-60 ℃, the washing time is 1-3 h, the solid-liquid mass ratio is 1:50-1:150, the washing end washing water PH is 7.0-7.8, the drying temperature is 100-150 ℃, the drying time is 1-4 h, further, the washing temperature is 35-50 ℃, the washing time is 1-2 h, the solid-liquid mass ratio is 1:70-1:100, the washing end washing water PH is 7.0-7.4, the drying temperature is 120-140 ℃, and the drying time is 1-2 h.
Compared with the traditional magnesium thermal reduction method, the method has the outstanding advantages that new metal impurities are not introduced in the process, the method has the outstanding advantages of source impurity reduction and process impurity control, the purity of the metal beryllium is obviously higher than that of the metal beryllium prepared by the magnesium thermal reduction method, the purity can at least reach more than 99.99 percent, and compared with the magnesium thermal method, the method can only obtain beryllium beads, and the nano-micro beryllium powder with more excellent physical properties can be directly obtained.
Drawings
FIG. 1 is a flow chart of a method for preparing ultra-high purity nano-grade metallic beryllium powder.
The application is further described below in connection with the detailed description.
Detailed Description
The present disclosure is described in further detail below with reference to the drawings and the embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant content and not limiting of the present disclosure. It should be further noted that, for convenience of description, only a portion relevant to the present disclosure is shown in the drawings.
In addition, embodiments of the present disclosure and features of the embodiments may be combined with each other without conflict. The technical aspects of the present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Unless otherwise indicated, the exemplary implementations/embodiments shown are to be understood as providing exemplary features of various details of some ways in which the technical concepts of the present disclosure may be practiced. Thus, unless otherwise indicated, features of the various implementations/embodiments may be additionally combined, separated, interchanged, and/or rearranged without departing from the technical concepts of the present disclosure.
Example 1
The embodiment provides a method for preparing ultra-high purity nano-grade metal beryllium powder. The method specifically comprises the following steps:
step a:500g of industrial-grade beryllium oxide is added into 3520g of 50% sodium hydroxide solution, the system temperature is controlled to be 90 ℃, after the beryllium oxide is completely dissolved in a stirring state, the reaction solution is added into 15 liters of pure water, the stirring state is heated to be 50 ℃, and when a large amount of white fine particles are precipitated in the solution, the solution is timely filtered by heat, so as to obtain 818g of high-purity beryllium hydroxide;
step b: adding high-purity beryllium hydroxide into 7840g of 20% high-purity sodium hydroxide solution, controlling the system temperature to be 50 ℃, and carrying out hot filtration through a high-precision filter element when the reaction liquid is completely clear to obtain high-purity sodium beryllium acid solution for heat preservation for later use;
step c: adding the high-purity sodium fluoberyllium acid solution into a 20-liter autoclave made of hastelloy material, introducing high-purity hydrogen to remove oxygen and controlling the hydrogen pressure at 150Kg/cm 2 Heating to 250deg.C under stirring, and pulse-type introducing hydrogen into the kettle (maintaining hydrogen partial pressure in the kettle not lower than 100 Kg/cm) 2 ) When the pressure in the autoclave was maintained substantially unchanged (recording pressure was 140Kg/cm 2 ) The hydrogen reduction reaction was completed and the time for hydrogen reduction was 3.2 hours. Under the condition of maintaining the system pressure and temperature, the hydrogen reduction slurry is quickly led into an online filter made of a Hash alloy material by relying on high-pressure gas action, and the solid-liquid quick separation is realized in the high-pressure hydrogen atmosphere;
step d: the powder obtained by separation is added into 10 liters of pure water, heated to 40 ℃ and washed for 1 hour, the filtration and separation are repeated for three times, and after the last filtration and separation, the pure water is used for in-situ washing until the pH of the leaching solution is 7.2. Transferring the washed powder material into a 50 liter double-cone rotary vacuum drier with enamel sprayed on the inner wall, and drying for 1h at 120 ℃ to obtain 146g gray ferrous beryllium powder.
Example 2
The embodiment provides a method for preparing ultra-high purity nano-grade metal beryllium powder. The method specifically comprises the following steps:
step a:700g of industrial-grade beryllium oxide is added into 4590g of 55% sodium hydroxide solution, the temperature of the system is controlled to be 100 ℃, after the beryllium oxide is completely dissolved in a stirring state, the reaction solution is added into 24 liters of pure water, the stirring state is heated to 70 ℃, and when a large amount of white fine particles are precipitated in the solution, the solution is timely filtered by heat, so that 1133g of high-purity beryllium hydroxide is obtained;
step b: adding high-purity beryllium hydroxide into 8853g of 25% high-purity sodium hydroxide solution, controlling the system temperature to 60 ℃, and carrying out hot filtration through a high-precision filter element when the reaction liquid is completely clear to obtain high-purity sodium beryllium acid solution for heat preservation for later use;
step c: adding the high-purity sodium fluoberyllium acid solution into a 20-liter autoclave made of hastelloy material, introducing high-purity hydrogen to remove oxygen and controlling the hydrogen pressure at 160Kg/cm 2 Heating to 280 ℃ under stirring, and introducing into the kettle in a pulse mannerHydrogen is introduced (the partial pressure of hydrogen in the kettle is maintained to be not lower than 105 Kg/cm) 2 ) When the pressure in the autoclave was maintained substantially unchanged (recording pressure was 169 Kg/cm) 2 ) The hydrogen reduction reaction was completed and the hydrogen reduction time was 2.8 hours. Under the condition of maintaining the system pressure and temperature, the hydrogen reduction slurry is quickly led into an online filter made of a Hash alloy material by relying on high-pressure gas action, and the solid-liquid quick separation is realized in the high-pressure hydrogen atmosphere;
step d: the powder obtained by separation is added into 16 liters of pure water, heated to 45 ℃ and washed for 1.5 hours, the filtration and separation are repeated for three times, and after the last filtration and separation, pure water is used for in-situ washing until the pH of the leaching solution is 7.1. Transferring the washed powder material into a 50 liter double-cone rotary vacuum drier with enamel sprayed on the inner wall, and drying for 1.5 hours at 130 ℃ to obtain 204g gray ferrous beryllium powder.
Example 3
The embodiment provides a method for preparing ultra-high purity nano-grade metal beryllium powder. The method specifically comprises the following steps:
step a:600g of industrial-grade beryllium oxide is added into 3575g of 60% sodium hydroxide solution, the system temperature is controlled to be 110 ℃, after the beryllium oxide is completely dissolved in a stirring state, the reaction solution is added into 21 liters of pure water, the stirring state is heated to be 70 ℃, and when a large amount of white fine particles are precipitated in the solution, the solution is timely filtered by heat, so as to obtain 976g of high-purity beryllium hydroxide;
step b: adding high-purity beryllium hydroxide into 9939g of 19% high-purity sodium hydroxide solution, controlling the system temperature to 60 ℃, and carrying out hot filtration through a high-precision filter element when the reaction liquid is completely clear to obtain high-purity sodium beryllium acid solution for heat preservation for later use;
step c: adding the high-purity sodium fluoberyllium acid solution into a 20-liter autoclave made of hastelloy material, introducing high-purity hydrogen to remove oxygen and controlling the hydrogen pressure at 165Kg/cm 2 Heating to 270 ℃ under stirring, and introducing hydrogen into the kettle in pulse mode (maintaining hydrogen partial pressure in the kettle not lower than 105 Kg/cm) 2 ) When the pressure in the autoclave was maintained substantially unchanged (recording pressure was 160Kg/cm 2 ) The hydrogen reduction reaction was completed, and the time for hydrogen reduction was 3.0 hours. Depending on the high-pressure gas action under the condition of maintaining the system pressure and temperatureThe hydrogen reduction slurry is quickly led into an online filter made of a Hash alloy material, and solid-liquid quick separation is realized in a high-pressure hydrogen atmosphere;
step d: the powder obtained by separation is added into 14 liters of pure water, heated to 50 ℃ and washed for 2 hours, the filtration and separation are repeated for three times, and after the last filtration and separation, pure water is used for in-situ washing until the pH of the leaching solution is 7.1. The washed powder material is transferred into a 50 liter double cone rotary vacuum drier with enamel sprayed on the inner wall, and is dried for 1.5 hours at 135 ℃ to obtain 175g gray ferrous beryllium powder.
Example 4
The embodiment provides a method for preparing ultra-high purity nano-grade metal beryllium powder. The method specifically comprises the following steps:
step a:1000g of industrial beryllium oxide is added into 62772 g of 60% sodium hydroxide solution, the system temperature is controlled to 120 ℃, after the beryllium oxide is completely dissolved in a stirring state, the reaction solution is added into 30 liters of pure water, the stirring state is heated to 80 ℃, and when a large amount of white fine particles are precipitated in the solution, the solution is timely filtered by heat, so that 1601g of high-purity beryllium hydroxide is obtained;
step b: adding high-purity beryllium hydroxide into 13945g of 22% high-purity sodium hydroxide solution, controlling the system temperature to be 50 ℃, and carrying out hot filtration through a high-precision filter element when the reaction liquid is completely clear to obtain high-purity sodium beryllium acid solution for heat preservation for later use;
step c: adding the high-purity sodium fluoberyllium acid solution into a 20-liter autoclave made of hastelloy material, introducing high-purity hydrogen to remove oxygen and controlling the hydrogen pressure at 175Kg/cm 2 Heating to 275 ℃ under stirring, and introducing hydrogen into the kettle in pulse mode (maintaining hydrogen partial pressure in the kettle not lower than 100 Kg/cm) 2 ) When the pressure in the autoclave was maintained substantially unchanged (recording pressure was 160Kg/cm 2 ) The hydrogen reduction reaction was completed, and the time for hydrogen reduction was 3.0 hours. Under the condition of maintaining the system pressure and temperature, the hydrogen reduction slurry is quickly led into an online filter made of a Hash alloy material by relying on high-pressure gas action, and the solid-liquid quick separation is realized in the high-pressure hydrogen atmosphere;
step d: the powder obtained by separation is added into 25 liters of pure water, heated to 45 ℃ and washed for 2 hours, the filtration and separation are repeated for three times, and after the last filtration and separation, pure water is used for in-situ washing until the pH of the leaching solution is 7.1. Transferring the washed powder material into a 50 liter double-cone rotary vacuum drier with enamel sprayed on the inner wall, and drying for 1h at 140 ℃ to obtain 287g gray ferrous beryllium powder.
Example 5
The embodiment provides a method for preparing ultra-high purity nano-grade metal beryllium powder. The method specifically comprises the following steps:
step a:900g of industrial-grade beryllium oxide is added into 6158g of 55% sodium hydroxide solution, the system temperature is controlled to be 100 ℃, after the beryllium oxide is completely dissolved in a stirring state, the reaction solution is added into 27 liters of pure water, the stirring state is heated to 80 ℃, and when a large amount of white fine particles are precipitated in the solution, the solution is timely filtered by heat, so as to obtain 1441g of high-purity beryllium hydroxide;
step b: adding high-purity beryllium hydroxide into 13940g of 20% high-purity sodium hydroxide solution, controlling the system temperature to 65 ℃, and carrying out hot filtration through a high-precision filter element when the reaction liquid is completely clear to obtain high-purity sodium beryllium acid solution for later use;
step c: adding the high-purity sodium fluoberyllium acid solution into a 20-liter autoclave made of hastelloy material, introducing high-purity hydrogen to remove oxygen and controlling the hydrogen pressure at 170Kg/cm 2 Heating to 285deg.C under stirring, and pulse-type introducing hydrogen into the kettle (maintaining hydrogen partial pressure in the kettle not lower than 100 Kg/cm) 2 ) When the pressure in the autoclave was maintained substantially unchanged (recording pressure was 169 Kg/cm) 2 ) The hydrogen reduction reaction was completed and the hydrogen reduction time was 2.7 hours. Under the condition of maintaining the system pressure and temperature, the hydrogen reduction slurry is quickly led into an online filter made of a Hash alloy material by relying on high-pressure gas action, and the solid-liquid quick separation is realized in the high-pressure hydrogen atmosphere;
step d: the powder obtained by separation is added into 22 liters of pure water, heated to 50 ℃ and washed for 1.5 hours, the filtration and separation are repeated for three times, and after the last filtration and separation, pure water is used for in-situ washing until the pH of the leaching solution is 7.2. Transferring the washed powder material into a 50 liter double-cone rotary vacuum drier with enamel sprayed on the inner wall, and drying for 1h at 140 ℃ to obtain 258g gray ferrous beryllium powder.
The metallic beryllium powder samples prepared in examples 1 to 5 were analyzed and the results are shown in table 1:
TABLE 1 analysis of samples of metallic beryllium powders prepared in examples 1 to 5
As can be seen from Table 1, the method adopts the sub-molten salt alkaline method to hydrolyze and purify to obtain high-purity beryllium hydroxide, and then combines the high-pressure hydrogen reduction method to prepare the metal beryllium powder, and the method has the advantages of easy control of technical process, low production cost and strong adaptability to raw materials. The metal beryllium powder prepared in the examples 1-5 has very high purity (more than 99.99%), very low impurity content, excellent chemical property of magnesium-free silicon-carbon-phosphorus ultra-low iron-nickel-oxygen, average particle size of powder particles of 1-2 mu m and all indexes completely meet the technical requirements of nano-micro ultra-high purity metal beryllium powder.
The method has strong adaptability to raw materials and low purity beryllium oxide, and the method is coupled with the raw material purification process, and no new impurity is introduced in the high-pressure hydrogen reduction process, so that the metal beryllium powder prepared by the method can reach ultra-high purity (the purity is more than 99.99%).
In the description of the present specification, reference to the terms "one embodiment/manner," "some embodiments/manner," "example," "a particular example," "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/manner or example is included in at least one embodiment/manner or example of the application. In this specification, the schematic representations of the above terms are not necessarily for the same embodiment/manner or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/modes or examples described in this specification and the features of the various embodiments/modes or examples can be combined and combined by persons skilled in the art without contradiction.
It will be appreciated by those skilled in the art that the above-described embodiments are merely for clarity of illustration of the disclosure, and are not intended to limit the scope of the disclosure. Other variations or modifications will be apparent to persons skilled in the art from the foregoing disclosure, and such variations or modifications are intended to be within the scope of the present disclosure.
Claims (8)
1. The preparation process of ultra-high purity nanometer level beryllium powder includes the following steps:
a. purifying beryllium oxide: heating and dissolving industrial-grade beryllium oxide in a high-concentration sodium hydroxide solution, adding the solution into pure water at a certain temperature to perform hydrolysis reaction to generate high-purity beryllium hydroxide, performing hot filtration to obtain high-purity beryllium hydroxide, evaporating and concentrating the hydrolysate to recover high-concentration alkali liquor, and recycling the hydrolysate for the dissolving process of industrial beryllium oxide;
b. preparing a high-purity sodium beryllium acid solution: heating and reacting high-purity beryllium hydroxide with excessive high-purity sodium hydroxide solution, and thermally filtering the reaction solution through a high-precision filter element to obtain high-purity sodium beryllium acid solution;
c. high pressure hydrogen reduction: introducing high-purity high-pressure hydrogen into a high-pressure reaction kettle made of special alloy materials to perform medium-temperature hydrothermal reduction reaction to generate nano-grade metal beryllium powder;
d. and (3) online separation: under the condition that the high-pressure hydrogen reduction slurry is kept in a reaction working condition, under the action of high-pressure pneumatic, the high-pressure hydrogen reduction slurry is quickly led into an online filter, solid-liquid quick separation is realized in a high-pressure hydrogen atmosphere, nano-micro metal beryllium powder is obtained, and the reduction solution is a high-purity sodium hydroxide solution and is circularly used for preparing the high-purity sodium beryllium acid solution;
e. purifying beryllium powder: washing, separating and dynamically drying the beryllium powder by multistage pure water to obtain the ultra-high purity nano-micro level metal beryllium powder.
2. The method of claim 1, wherein the ultra-high purity nano-micro grade metal beryllium powder comprises Si, al, mg, fe, cu, ni, cr, pb, mn, co, zn, cd, li, ag, B, sm, eu, gd, dy, ca, ba, sr, ti, V, W, mo, zr, se, Y, nb, K, na, C, P, O impurities, the sum of the impurities is not more than 100ppm, wherein most of the impurities are not detected, the purity is above 4N, and the average particle size of the beryllium powder is between 0.5 and 5 μm.
3. The method according to claim 1 or 2, wherein the industrial-grade beryllium oxide in the step a is beryllium oxide with purity lower than 99%, the dissolution temperature of the beryllium oxide is 80-150 ℃, the concentration of sodium hydroxide solution is 35-85%, the molar ratio of the beryllium oxide to the sodium hydroxide is 1:2.05-1:2.50, the hydrolysis reaction temperature is 30-90 ℃, and the mass ratio of the beryllium oxide to the pure water is 1:15-1:50.
4. The process according to claim 1 or 2, wherein in step b the reaction temperature is 30-80 ℃, the molar ratio of beryllium hydroxide to sodium hydroxide is 1:2.02-1:2.20, the concentration of sodium hydroxide solution is 10-30%, high purity sodium hydroxide means that the total contains Al, fe, cu, cr, pb, mn, co, zn, cd, ag, ti, V, W, mo, zr, se, Y, nb impurities, the sum of which is not more than 50ppm.
5. The process according to claim 1 or 2, wherein in step c the hydrogen reduction temperature is 200-350 ℃, the reaction time is 2-10 h, the hydrogen is pulsed, the hydrogen pressure is 50-200 Kg/cm 2 The purity of the hydrogen is 5N, and the special alloy material is nickel-based alloy material.
6. The method of claim 5, wherein the nickel-based alloy material is hastelloy or Meng Naer alloy.
7. The process according to claim 1 or 2, wherein in step d, the in-line separation temperature is 200 to 300 ℃ and the hydrogen pressure is 100 to 160Kg/cm 2 。
8. The method according to claim 1 or 2, wherein the washing temperature of beryllium powder in step e is 25-60 ℃, the washing time is 1-3 h, the solid-liquid mass ratio is 1:50-1:150, the washing mode adopts multistage pure water pulping washing combined with in-situ washing, the washing end point washing water PH is 7.0-7.8, the drying temperature is 100-150 ℃, the drying time is 1-4 h, and the drying mode adopts double cone rotary vacuum drying.
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