CN111455406A - Preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium - Google Patents
Preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium Download PDFInfo
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- CN111455406A CN111455406A CN202010277893.XA CN202010277893A CN111455406A CN 111455406 A CN111455406 A CN 111455406A CN 202010277893 A CN202010277893 A CN 202010277893A CN 111455406 A CN111455406 A CN 111455406A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F3/00—Compounds of beryllium
Abstract
The technical scheme of the invention provides a preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium, wherein the preparation method of the high-purity beryllium chloride comprises the following steps: fully mixing beryllium oxide, charcoal, tar and water according to a certain proportion, briquetting, and calcining and coking under the protection of inert gas to obtain a coking material; placing the coking material in a chlorination system, introducing chlorine into the chlorination system, reacting the coking material with the chlorine, and collecting the generated crude beryllium chloride; and transferring the crude beryllium chloride into a distillation-condensation system, introducing nitrogen into the distillation-condensation system, and extracting and collecting high-purity beryllium chloride by adopting a distillation method. The technical scheme of the invention takes the high-purity beryllium chloride as a raw material, and the purity of the nuclear pure-grade metal beryllium prepared by a molten salt electrolysis method can at least reach 99.9 percent and even more than 99.95 percent.
Description
Technical Field
The invention relates to the field of high-purity preparation of organic reaction catalysts, in particular to a preparation method of high-purity beryllium chloride, further relates to the field of rare metal pyrogenic process-molten salt electrolysis coupling metallurgy, and in particular relates to a preparation method of nuclear pure-grade metal beryllium which is a key raw material in national defense industry.
Background
Beryllium has excellent nuclear performance, thermal performance and optical performance, is known as new nuclear metal, has extremely important application in the fields of advanced national defense science and technology and aerospace, and is an important ring for developing advanced national defense technology and strategic emerging industry and an important research object for national strategic resource utilization and storage.
Beryllium is applied to the departments of machinery, electronics, petroleum, chemical engineering, traffic, national defense industry and the like in the forms of beryllium copper, beryllium aluminum, beryllium nickel alloy, nuclear pure metal beryllium, beryllium oxide and the like. The metallic beryllium, particularly the nuclear pure-grade beryllium, has small density, high strength and excellent nuclear performance, and is widely used as a structural material of missiles and satellites and an inertial navigation system, and also as a structural material of nuclear reactors and nuclear weapons and a neutron source material. The metallic beryllium is prepared by a magnesium thermal reduction method, and the purity of the beryllium prepared by the method is low and cannot reach the nuclear purity level, so that the application of the metallic beryllium in the field of aerospace is limited.
Disclosure of Invention
In view of the above-mentioned prior art, the technical problem to be solved by the present invention is to provide a method for preparing high-purity beryllium chloride and nuclear-pure metallic beryllium.
In the present invention, the term "high-purity beryllium chloride" means that Na is included+、K+、Ca2+、Mg2+、Cl－These 25 impurity levels, together, do not exceed 200ppm, with the respective key impurity levels (e.g., B, Hg, etc.) not exceeding 1 ppm.
The 'nuclear pure grade metal beryllium' in the invention is Na+、K+、Ca2+、Mg2+、Cl－Equal 25 impurity levels, totaling no more than 1000ppm, more preferably, totaling no more than 300ppm, with each key impurity level (e.g., B, Hg, etc.) not exceeding 1 ppm.
In order to solve the technical problems, the technical scheme of the invention provides a preparation method of high-purity beryllium chloride, which comprises the following steps:
1) fully mixing beryllium oxide, charcoal, tar and water according to a certain proportion, briquetting, and calcining and coking under the protection of inert gas to obtain a coking material;
2) placing the coking material in a chlorination system, introducing chlorine into the chlorination system, reacting the coking material with the chlorine, and collecting the generated crude beryllium chloride;
3) and transferring the crude beryllium chloride into a distillation-condensation system, introducing nitrogen into the distillation-condensation system, and extracting and collecting high-purity beryllium chloride by adopting a distillation method.
Preferably, in the step 1), the mass ratio of beryllium oxide, charcoal, tar and water is 1 (0.6-1.5) to (0.7-1.4): (0.9-1.6). Further preferably, the mixing ratio is 1 (1.0-1.3) to 0.9-1.2): (0.9-1.2).
Preferably, in the step 1), the coking temperature is 600-1100 ℃, and the coking time is 6-15 h. Further preferably, the coking temperature is 800-1000 ℃, and the coking time is 9-12 h.
Preferably, in the step 2), the chlorination system comprises a chlorination section and a condensation collection section, wherein the chlorination section performs chlorination reaction, the condensation collection section collects crude beryllium chloride, the chlorination temperature is 500-1000 ℃, the chlorination time is 8-15 h, the chlorine flow is 1L/min-5L/min, further, the chlorination temperature is 600-800 ℃, the chlorination time is 10-13 h, and the chlorine flow is 2-4L/min, and preferably, high-purity chlorine is selected.
Preferably, in the step 3), the distillation temperature is 600-1000 ℃, the distillation time is 5-10 h, and the nitrogen flow is 2L-10L/min, further, the distillation temperature is 650-800 ℃, the distillation time is 7-9 h, and the high-purity nitrogen flow is 4-7L/min.
In order to solve the technical problems, the technical scheme of the invention also provides a preparation method of nuclear pure-grade metal beryllium, which adopts the preparation method of high-purity beryllium chloride and comprises the following steps:
1) mixing the high-purity beryllium chloride with sodium chloride to form a mixed salt;
2) electrolyzing the mixed salt by adopting a melting electrolysis method;
3) and collecting the separated solid substance, and performing post-treatment to obtain the nuclear pure-grade metal beryllium.
Preferably, in the step 1), the mass ratio of the high-purity beryllium chloride to the sodium chloride is 1: (1-1.2).
Preferably, in the step 2), the mixed salt is placed in a graphite crucible, and the molten electrolysis is carried out by taking a plurality of metal nickel sheets connected in parallel as a cathode and the graphite crucible as an anode.
Preferably, the electrolysis temperature is 300-500 ℃, and the electrolysis time is 1-4 h. More preferably, the electrolysis temperature is 300-400 ℃, and the electrolysis time is 2-3 h.
Preferably, in the step 3), the cathode is taken out, crude beryllium is obtained by stripping, and the nuclear pure-grade metal beryllium is obtained by washing and drying with pure water. The drying temperature of the metal beryllium is 80-150 ℃, the drying time is 3-6 h, further, the drying temperature is 100-120 ℃, and the drying time is 4-6 h.
Compared with the traditional magnesium thermal reduction method, the method for preparing the nuclear pure-grade metal beryllium by adopting the high-purity organic synthesis catalyst, namely the anhydrous beryllium chloride and the molten salt electrolysis coupling technology of the beryllium chloride has the advantages that the purity of the metal beryllium is obviously higher than that of the metal beryllium prepared by the magnesium thermal reduction method because no new metal impurities are introduced in the process, and the purity of the metal beryllium can at least reach 99.9 percent and even more than 99.95 percent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a flow chart of a method for preparing high-purity beryllium chloride and nuclear pure-grade metallic beryllium according to the technical scheme of the invention.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
As shown in fig. 1, the preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium according to the technical scheme of the invention comprises the following steps:
1) fully mixing beryllium oxide, charcoal, tar and water according to a certain proportion, briquetting, and calcining and coking under the protection of inert gas to obtain a coking material;
2) placing the coking material in a chlorination system, introducing chlorine (preferably high-purity chlorine) into the chlorination system, reacting the coking material with the chlorine, and collecting the generated crude beryllium chloride;
3) and transferring the crude beryllium chloride to a distillation-condensation system, introducing nitrogen (preferably high-purity nitrogen), and extracting and collecting the high-purity beryllium chloride by a distillation method.
With reference to fig. 1, the nuclear pure-grade metallic beryllium is prepared by using the high-purity beryllium chloride, and the preparation method comprises the following steps:
1) mixing the high-purity beryllium chloride with sodium chloride (preferably high-purity sodium chloride) to form a mixed salt;
2) electrolyzing the mixed salt by adopting a melting electrolysis method;
3) and (3) collecting (stripping) separated solid matters, and performing post-treatment (washing and drying) to obtain the nuclear pure-grade metal beryllium.
Example 1
The preparation method of the high-purity beryllium chloride and the nuclear pure-grade metal beryllium comprises the following steps:
1) fully and uniformly mixing 700 g of industrial-grade beryllium oxide, 800 g of charcoal, 850 g of tar and 1000 g of water, briquetting in a special mould, introducing nitrogen into a tubular furnace, and heating and coking at 1000 ℃ for 11 hours to obtain a coking material;
2) the coking material is subjected to chlorination-condensation collection in a chlorination system, chlorinated for 10h at 850 ℃ under the condition of introducing high-purity chlorine gas of 4L/min, and collected in a glove box to obtain 1086 g of crude beryllium chloride;
3) transferring the crude beryllium chloride into a distillation-condensation purification system in a glove box, distilling for 8 hours at 800 ℃ under the condition of introducing high-purity nitrogen of 6L/min, and collecting 999 g of high-purity beryllium chloride in the glove box.
And then the nuclear pure-grade metal beryllium is prepared by adopting the high-purity beryllium chloride, and the preparation method comprises the following steps:
1) taking 900 g of high-purity beryllium chloride and 900 g of high-purity sodium chloride respectively from a glove box, and uniformly mixing the high-purity beryllium chloride and the high-purity sodium chloride in a graphite crucible;
2) a plurality of metal nickel sheets connected in parallel are used as cathodes, a graphite crucible is used as an anode, and the electrolysis is carried out for 2.5 hours in a molten salt state after the temperature is raised to 350 ℃;
3) after electrolysis, the cathode nickel sheet is taken out, peeled to obtain crude crystalline beryllium, washed by pure water and dried at 120 ℃ for 4 hours to obtain 66 g of nuclear pure metallic beryllium.
Example 2
The preparation method of the high-purity beryllium chloride and the nuclear pure-grade metal beryllium comprises the following steps:
1)500 g of industrial-grade beryllium oxide, 600 g of charcoal, 550 g of tar and 700 g of water are fully and uniformly mixed, then the mixture is pressed into a special die, then nitrogen is introduced into a tube furnace, and the mixture is heated and coked for 10 hours at 900 ℃ to obtain a coking material;
2) the coking material is subjected to chlorination-condensation collection in a chlorination system, chlorinated for 11h at 800 ℃ under the condition of introducing high-purity chlorine gas of 3L/min, and collected in a glove box to obtain 706 g of crude beryllium chloride;
3) the crude beryllium chloride is transferred into a distillation-condensation purification system in a glove box, distilled for 6 hours at 700 ℃ under the condition of introducing high-purity nitrogen of 5L/min, and collected in the glove box to obtain 635 g of high-purity beryllium chloride.
And then the nuclear pure-grade metal beryllium is prepared by adopting the high-purity beryllium chloride, and the preparation method comprises the following steps:
1) taking 600 g of high-purity beryllium chloride and 600 g of high-purity sodium chloride respectively from a glove box, and uniformly mixing the high-purity beryllium chloride and the high-purity sodium chloride in a graphite crucible;
2) a plurality of metal nickel sheets connected in parallel are used as cathodes, a graphite crucible is used as an anode, and the electrolysis is carried out for 2 hours in a molten salt state after the heating to 400 ℃;
3) after electrolysis, the cathode nickel sheet is taken out, peeled to obtain crude crystalline beryllium, washed by pure water and dried at 110 ℃ for 3 hours to obtain 47.5 g of nuclear pure metallic beryllium.
Example 3
The preparation method of the high-purity beryllium chloride and the nuclear pure-grade metal beryllium comprises the following steps:
1) fully and uniformly mixing 600 g of industrial-grade beryllium oxide, 750 g of charcoal, 600 g of tar and 850 g of water, briquetting in a special mould, introducing nitrogen into a tubular furnace, and heating and coking at 900 ℃ for 12 hours to obtain a coking material;
2) the coking material is subjected to chlorination-condensation collection in a chlorination system, chlorinated for 13h at 900 ℃ under the condition of introducing high-purity chlorine gas of 2.5L/min, and collected in a glove box to obtain 978 g of crude beryllium chloride;
3) the crude beryllium chloride is transferred into a distillation-condensation purification system in a glove box, distilled for 8 hours at 850 ℃ under the condition of introducing high-purity nitrogen of 4L/min, and collected in the glove box to obtain 880 g of high-purity beryllium chloride.
And then the nuclear pure-grade metal beryllium is prepared by adopting the high-purity beryllium chloride, and the preparation method comprises the following steps:
1) taking 800 g of high-purity beryllium chloride and 800 g of high-purity sodium chloride respectively from a glove box, and uniformly mixing the high-purity beryllium chloride and the high-purity sodium chloride in a graphite crucible;
2) a plurality of metal nickel sheets connected in parallel are used as cathodes, a graphite crucible is used as an anode, and the electrolysis is carried out for 3 hours in a molten salt state after the temperature is increased to 370 ℃;
3) after electrolysis, the cathode nickel sheet is taken out, peeled to obtain crude crystalline beryllium, washed by pure water and dried at 110 ℃ for 3 hours to obtain 62.1 g of nuclear pure metallic beryllium.
Example 4
The preparation method of the high-purity beryllium chloride and the nuclear pure-grade metal beryllium comprises the following steps:
1) fully and uniformly mixing 400 g of industrial-grade beryllium oxide, 450 g of charcoal, 450 g of tar and 550 g of water, briquetting in a special mould, introducing nitrogen into a tube furnace, and heating and coking at 800 ℃ for 14h to obtain a coking material;
2) the coking material is subjected to chlorination-condensation collection in a chlorination system, chlorinated for 12 hours at 750 ℃ under the condition of introducing high-purity chlorine gas of 4L/min, and collected in a glove box to obtain 640 g of crude beryllium chloride;
3) the crude beryllium chloride is transferred into a distillation-condensation purification system in a glove box, distilled for 7 hours at 750 ℃ under the condition of introducing high-purity nitrogen of 5L/min, and collected in the glove box to obtain 589 g of high-purity beryllium chloride.
And then the nuclear pure-grade metal beryllium is prepared by adopting the high-purity beryllium chloride, and the preparation method comprises the following steps:
(1) taking 500 g of high-purity beryllium chloride and 500 g of high-purity sodium chloride respectively from a glove box, and uniformly mixing the high-purity beryllium chloride and the high-purity sodium chloride in a graphite crucible;
(2) a plurality of metal nickel sheets connected in parallel are used as cathodes, a graphite crucible is used as an anode, and the electrolysis is carried out for 2 hours in a molten salt state after the heating to 400 ℃;
3) after electrolysis, the cathode nickel sheet is taken out, peeled to obtain crude crystalline beryllium, washed by pure water and dried at 115 ℃ for 3 hours to obtain 41.6 g of nuclear pure metallic beryllium.
Example 5
The preparation method of the high-purity beryllium chloride and the nuclear pure-grade metal beryllium comprises the following steps:
1) fully and uniformly mixing 800 g of industrial-grade beryllium oxide, 900 g of charcoal, 1000 g of tar and 1200 g of water, briquetting in a special mould, introducing nitrogen into a tubular furnace, and heating and coking at 950 ℃ for 12 hours to obtain a coking material;
2) the coking material is subjected to chlorination-condensation collection in a chlorination system, chlorinated for 12 hours at 900 ℃ under the condition of introducing high-purity chlorine gas of 5L/min, and collected in a glove box to obtain 1316 g of crude beryllium chloride;
3) transferring the crude beryllium chloride into a distillation-condensation purification system in a glove box, distilling for 8 hours at 800 ℃ under the condition of introducing high-purity nitrogen of 6L/min, and collecting 1198 g of high-purity beryllium chloride in the glove box.
And then the nuclear pure-grade metal beryllium is prepared by adopting the high-purity beryllium chloride, and the preparation method comprises the following steps:
(1) taking 1100 g of high-purity beryllium chloride and 1100 g of high-purity sodium chloride respectively from a glove box, and uniformly mixing the high-purity beryllium chloride and the high-purity sodium chloride in a graphite crucible;
(2) a plurality of metal nickel sheets connected in parallel are used as cathodes, a graphite crucible is used as an anode, and the electrolysis is carried out for 2 hours in a molten salt state after the temperature is raised to 350 ℃;
3) after electrolysis, the cathode nickel sheet is taken out, peeled to obtain crude crystalline beryllium, washed by pure water and dried at 130 ℃ for 4 hours to obtain 80.4 g of nuclear pure metallic beryllium.
The results of analyzing the nuclear pure grade beryllium metal samples prepared in examples 1 to 5 are shown in table 1:
TABLE 1 analysis of nuclear pure grade metallic beryllium samples
As can be seen from Table 1, the invention adopts a coking-chlorination-distillation purification method to prepare high-purity beryllium chloride, and combines a beryllium chloride-sodium chloride molten salt electrolysis method to prepare nuclear-pure-grade metal beryllium, and the method has the advantages of easy control of process, low production cost and strong adaptability to raw materials. The metal beryllium prepared in the embodiments 1-5 has high main content, high purity (more than 99.95%), low impurity content and stable quality, and all indexes completely meet the technical requirements of nuclear purity grade.
While specific embodiments of the present invention have been described in detail above, it will be appreciated that those skilled in the art, upon attaining an understanding of the foregoing may readily produce alterations to, variations of, and equivalents to these embodiments. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A preparation method of high-purity beryllium chloride is characterized by comprising the following steps:
1) fully mixing beryllium oxide, charcoal, tar and water according to a certain proportion, briquetting, and calcining and coking under the protection of inert gas to obtain a coking material;
2) placing the coking material in a chlorination system, introducing chlorine into the chlorination system, reacting the coking material with the chlorine, and collecting the generated crude beryllium chloride;
3) and transferring the crude beryllium chloride into a distillation-condensation system, introducing nitrogen into the distillation-condensation system, and extracting and collecting high-purity beryllium chloride by adopting a distillation method.
2. The method for preparing beryllium chloride as claimed in claim 1, wherein in the step 1), the mass ratio of beryllium oxide, charcoal, tar and water is 1 (0.6-1.5) to (0.7-1.4): (0.9-1.6).
3. The method for preparing beryllium chloride of claim 1, wherein in step 1), the coking temperature is 600 ℃ to 1100 ℃ and the coking time is 6h to 15 h.
4. The method for preparing beryllium chloride as claimed in claim 1, wherein in the step 2), the chlorination system comprises a chlorination section and a condensation collection section, the chlorination section performs chlorination reaction, the condensation collection section collects crude beryllium chloride, the chlorination temperature is 500-1000 ℃, the chlorination time is 8-15 h, and the chlorine flow rate is 1L/min-5L/min.
5. The method for preparing beryllium chloride as claimed in claim 1, wherein in step 3), the distillation temperature is 600 ℃ to 1000 ℃, the distillation time is 5h to 10h, and the nitrogen flow rate is 2L/min to 10L/min.
6. A method for preparing nuclear-pure metallic beryllium, which is characterized by adopting the high-purity beryllium chloride of any one of claims 1 to 5 and comprises the following steps:
1) mixing the high-purity beryllium chloride with sodium chloride to form a mixed salt;
2) electrolyzing the mixed salt by adopting a melting electrolysis method;
3) and collecting the separated solid substance, and performing post-treatment to obtain the nuclear pure-grade metal beryllium.
7. The method according to claim 6, wherein in step 1), the mass ratio of the high-purity beryllium chloride to the sodium chloride is 1: (1-1.2).
8. The method according to claim 6 or 7, wherein in the step 2), the mixed salt is placed in a graphite crucible, and the molten electrolysis is performed with a plurality of metallic nickel sheets connected in parallel as a cathode and the graphite crucible as an anode.
9. The method according to claim 8, wherein the electrolysis temperature is 300 to 500 ℃ and the electrolysis time is 1 to 4 hours.
10. The preparation method according to claim 8, wherein in step 3), the cathode is taken out, crude beryllium is obtained by stripping, and nuclear pure-grade metallic beryllium is obtained by washing with pure water and drying.
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| CN112357885A (en) * | 2020-12-02 | 2021-02-12 | 中国科学院上海应用物理研究所 | Purification method of single component in chloride molten salt |
| CN112813288A (en) * | 2020-12-29 | 2021-05-18 | 东方电气集团科学技术研究院有限公司 | Method for preparing high-purity beryllium from industrial beryllium |
| CN112981461A (en) * | 2021-02-05 | 2021-06-18 | 西藏智材新材料有限公司 | High-purity metal beryllium and preparation process thereof |
| CN113860338A (en) * | 2021-11-01 | 2021-12-31 | 上海翰军实验设备有限公司 | Preparation and purification device and method for high-purity anhydrous beryllium chloride |
| CN115305504A (en) * | 2021-05-08 | 2022-11-08 | 中南大学 | Method for preparing metal beryllium by fused salt electrolysis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112357885A (en) * | 2020-12-02 | 2021-02-12 | 中国科学院上海应用物理研究所 | Purification method of single component in chloride molten salt |
| CN112813288A (en) * | 2020-12-29 | 2021-05-18 | 东方电气集团科学技术研究院有限公司 | Method for preparing high-purity beryllium from industrial beryllium |
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| CN115305504A (en) * | 2021-05-08 | 2022-11-08 | 中南大学 | Method for preparing metal beryllium by fused salt electrolysis |
| CN113860338A (en) * | 2021-11-01 | 2021-12-31 | 上海翰军实验设备有限公司 | Preparation and purification device and method for high-purity anhydrous beryllium chloride |
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Application publication date: 20200728 |