CN111422890A - Preparation method of high-purity beryllium hydroxide and nuclear pure-grade beryllium oxide - Google Patents
Preparation method of high-purity beryllium hydroxide and nuclear pure-grade beryllium oxide Download PDFInfo
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- CN111422890A CN111422890A CN202010278041.2A CN202010278041A CN111422890A CN 111422890 A CN111422890 A CN 111422890A CN 202010278041 A CN202010278041 A CN 202010278041A CN 111422890 A CN111422890 A CN 111422890A
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Abstract
The technical scheme of the invention provides a preparation method of high-purity beryllium hydroxide and nuclear pure-grade beryllium oxide, wherein the high-purity beryllium hydroxide comprises the following steps: dissolving industrial-grade beryllium oxide in a sodium hydroxide solution; adding the dissolved solution into pure water to perform hydrolysis reaction; after the reaction is finished, performing centrifugal separation, wherein the solid beryllium hydroxide is washed and dried by pure water to obtain high-purity beryllium hydroxide; and (4) evaporating and concentrating the separated liquid, and circularly using the separated liquid for dissolving industrial-grade beryllium oxide. The nuclear pure-grade beryllium oxide can be obtained by using the high-purity beryllium hydroxide as a raw material and adopting a clean closed calcination mode. The technical scheme of the invention has strong adaptability of raw materials, and can prepare high-purity raw materials meeting the requirements of nuclear pure beryllium series products.
Description
Technical Field
The invention relates to the field of high-purity preparation of nuclear industry basic raw materials, in particular to a preparation method of high-purity beryllium hydroxide and nuclear pure-grade beryllium oxide.
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. The main products of the beryllium industrial chain comprise beryllium compounds (beryllium hydroxide, beryllium oxide, anhydrous beryllium fluoride, beryllium sulfate, beryllium acetate and the like), metallic beryllium, beryllium alloys, beryllium oxide ceramics and metallic beryllium-based composite materials, and the most important of the industrial chain are nuclear pure metallic beryllium, nuclear pure beryllium fluoride and nuclear pure beryllium oxide. The nuclear pure-grade beryllium oxide is mainly used for producing beryllium oxide ceramics, has high refractoriness, high thermal conductivity, good nuclear performance and excellent electrical performance, and is applied to high-grade refractory materials (such as crucibles for smelting refractory metals and the like), various high-power electronic devices and integrated circuits, nuclear reactor protective layers and neutron shielding layers.
An important prerequisite for obtaining these key materials is the necessity to produce beryllium hydroxide which meets the requirements of nuclear purity. The main methods for preparing high-purity beryllium hydroxide at present are a recrystallization method, a complex precipitation method, an ammonium acetate thermal decomposition method and the like, and in the purification methods, the purity of the beryllium hydroxide can only reach 99.9 percent generally, and the key technical index can hardly reach the requirement of 0.6 ppm.
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 hydroxide and nuclear pure-grade beryllium oxide.
In the present invention, the term "high-purity beryllium hydroxide" means that Na is included+、K+、Ca2+、Mg2+、
The 24 impurity levels, together, do not exceed 600ppm, with the respective key impurity levels (e.g., B, Hg, etc.) not exceeding 0.6 ppm.
The 'nuclear pure beryllium oxide' in the invention is characterized by comprising Na+、K+、Ca2+、Mg2+、
The 24 impurity levels, together not exceeding 1000ppm, with the respective key impurity levels (e.g., B, Hg, L i, 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 hydroxide, which comprises the following steps:
1) dissolving industrial-grade beryllium oxide in a sodium hydroxide solution;
2) adding the dissolved solution into pure water to perform hydrolysis reaction;
3) after the reaction is finished, performing centrifugal separation, wherein the solid beryllium hydroxide is washed and dried by pure water to obtain high-purity beryllium hydroxide; and (3) evaporating and concentrating the separated liquid, and circularly dissolving the industrial-grade beryllium oxide in the step 1).
Preferably, in the step 1), the temperature of the dissolving process is 120-200 ℃. Further preferably, the dissolving temperature is 150-180 ℃.
Preferably, in the step 1), the molar ratio of the sodium hydroxide to the industrial-grade beryllium oxide is (2-8): 1. Further preferably, the molar ratio of the sodium hydroxide to the industrial-grade beryllium oxide is (4-6): 1.
Preferably, in the step 1), the mass fraction of the sodium hydroxide is 60-90%. More preferably 75 to 85%, still more preferably 78 to 82%.
Preferably, in the step 2), the temperature of the hydrolysis reaction is 25-90 ℃. Furthermore, the hydrolysis temperature is 45-60 ℃.
Preferably, in the step 2), the volume ratio of the pure water to the dissolving solution is (10-20): 1. Preferably (12-15): 1.
Preferably, in the step 3), the mass ratio of pure water to solid beryllium hydroxide in the washing process is (8-16): 1, the washing time is 1-3 h, the temperature in the drying process is 70-150 ℃, and the drying time is 2-6 h. Furthermore, the mass ratio of pure water to solid beryllium hydroxide in the washing process is (10-13): 1, the washing time is 1-2 h, the temperature in the drying process is 100-120 ℃, and the drying time is 3-5 h.
Preferably, in the step 3), the mass fraction of the solute of the separation liquid after evaporation and concentration is 60-90%. More preferably 75 to 85%, still more preferably 78 to 82%.
In order to solve the technical problems, the technical scheme of the invention also provides a preparation method of nuclear pure beryllium oxide, which is prepared by calcining the high-purity beryllium hydroxide in a clean calcining-high-temperature beryllium dust recycling system which is closed in the whole process.
Preferably, the calcining temperature is 900-1200 ℃, the calcining time is 8-15 h, and the part of the calcining furnace contacting the materials is made of high-purity quartz or high-purity corundum materials. More preferably, the calcination temperature is 950-1050 ℃ and the calcination time is 10-12 h.
The traditional alkali dissolution-hydrolysis method only adopts low-purity beryllium hydroxide as a raw material, but the technical scheme of the invention is also suitable for low-activity low-purity beryllium oxide, has strong raw material adaptability, and can prepare high-purity raw materials meeting the requirements of nuclear pure-grade beryllium series products.
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 hydroxide and nuclear pure-grade beryllium oxide 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 hydroxide according to the technical scheme of the invention comprises the following steps:
1) dissolving industrial-grade beryllium oxide in a sodium hydroxide solution;
2) adding the dissolved solution into pure water to perform hydrolysis reaction;
3) after the reaction is finished, performing centrifugal separation, wherein the solid beryllium hydroxide is washed and dried by pure water to obtain high-purity beryllium hydroxide; and (3) evaporating and concentrating the separated liquid, and circularly dissolving the industrial-grade beryllium oxide in the step 1).
And continuing to refer to fig. 1, calcining the high-purity beryllium hydroxide in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process to obtain the nuclear pure-grade beryllium oxide.
Example 1
The preparation method of the high-purity beryllium hydroxide and the nuclear pure-grade beryllium oxide comprises the following steps:
1)1000 g of 95% beryllium oxide is gradually added into 5 kg of 85% sodium hydroxide high-concentration liquid, the process temperature is controlled to be 170-180 ℃, and the dissolution reaction process of industrial beryllium oxide is carried out;
2) adding the dissolved solution into pure water with the temperature of 60L 60 ℃ to perform hydrolysis reaction to generate beryllium hydroxide;
3) and carrying out centrifugal separation, washing with 10-12 times of pure water for 1.5h, and drying at 110 ℃ for 3h to obtain 1625 g of high-purity beryllium hydroxide. And the hydrolysate is dilute sodium hydroxide alkali liquor, is evaporated and concentrated to more than 80 percent, and is recycled for the dissolution reaction process of the industrial beryllium oxide.
Then, calcining the high-purity beryllium hydroxide in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process for 10 hours at 1000 ℃ to obtain 935 g of nuclear pure-grade beryllium oxide.
Example 2
The preparation method of the high-purity beryllium hydroxide and the nuclear pure-grade beryllium oxide comprises the following steps:
1)1200 g of 98% beryllium oxide is gradually added into 6.5 kg of 80% sodium hydroxide high-concentration liquid, the process temperature is controlled to be 170-175 ℃, and the dissolution reaction process of industrial beryllium oxide is generated;
2) adding the dissolved solution into pure water with the temperature of 90L 50 ℃ to perform hydrolysis reaction to generate beryllium hydroxide;
3) and (3) carrying out centrifugal separation, washing for 1h by using pure water with the volume being 12-13 times that of the pure water, and drying for 5h at the temperature of 100 ℃ to obtain 1982 g of high-purity beryllium hydroxide. And the hydrolysate is dilute sodium hydroxide alkali liquor, is evaporated and concentrated to more than 80 percent, and is recycled for the dissolution reaction process of the industrial beryllium oxide.
Then, calcining the high-purity beryllium hydroxide for 9 hours at 1050 ℃ in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process to obtain 1135 g of nuclear pure-grade beryllium oxide.
Example 3
The preparation method of the high-purity beryllium hydroxide and the nuclear pure-grade beryllium oxide comprises the following steps:
1) gradually adding 900 g of 96% beryllium oxide into 5.5 kg of 82% sodium hydroxide high-concentration liquid, controlling the process temperature to be 175-180 ℃, and carrying out a dissolution reaction process of industrial beryllium oxide;
2) adding the dissolved solution into pure water at 70L 55 ℃ to perform hydrolysis reaction to generate beryllium hydroxide;
3) and (3) carrying out centrifugal separation, washing for 1h by 14-15 times of pure water, and drying for 3h at 120 ℃ to obtain 1471 g of high-purity beryllium hydroxide. And the hydrolysate is dilute sodium hydroxide alkali liquor, is evaporated and concentrated to more than 80 percent, and is recycled for the dissolution reaction process of the industrial beryllium oxide.
Then, calcining the high-purity beryllium hydroxide for 12 hours at 960 ℃ in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process to obtain 838 g of nuclear pure-grade beryllium oxide.
Example 4
The preparation method of the high-purity beryllium hydroxide and the nuclear pure-grade beryllium oxide comprises the following steps:
1)1500 g of 95% beryllium oxide is gradually added into 11.5 kg of 78% sodium hydroxide high-concentration liquid, the process temperature is controlled to be 165-170 ℃, and the dissolution reaction process of industrial beryllium oxide is carried out;
2) adding the dissolved solution into pure water with the temperature of 160L 65 ℃ for hydrolysis reaction to generate beryllium hydroxide;
3) and (3) carrying out centrifugal separation, washing for 1.2h by 13-14 times of pure water, and drying for 4h at 115 ℃ to obtain 2400 g of high-purity beryllium hydroxide. And the hydrolysate is dilute sodium hydroxide alkali liquor, is evaporated and concentrated to more than 75%, and is recycled for the dissolution reaction process of the industrial beryllium oxide.
Then, calcining the high-purity beryllium hydroxide for 11 hours at 1000 ℃ in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process to obtain 1381 g of nuclear pure-grade beryllium oxide.
Example 5
The preparation method of the high-purity beryllium hydroxide and the nuclear pure-grade beryllium oxide comprises the following steps:
1)1400 g of 98% beryllium oxide is gradually added into 9 kg of 80% sodium hydroxide high-concentration liquid, the process temperature is controlled to be 170-175 ℃, and the dissolution reaction process of industrial beryllium oxide is generated;
2) adding the dissolved solution into pure water with the temperature of 110L 60 ℃ for hydrolysis reaction to generate beryllium hydroxide;
3) and (3) carrying out centrifugal separation, washing for 1.5h by 15-16 times pure water, and drying for 5h at 105 ℃ to obtain 2340 g of high-purity beryllium hydroxide. And the hydrolysate is dilute sodium hydroxide alkali liquor, is evaporated and concentrated to more than 80 percent, and is recycled for the dissolution reaction process of the industrial beryllium oxide.
Then, calcining the high-purity beryllium hydroxide for 13 hours at 980 ℃ in a clean calcining-high-temperature beryllium dust recovery system which is closed in the whole process to obtain 1324 g of nuclear pure-grade beryllium oxide.
The results of analyzing the nuclear pure beryllium oxide samples prepared in examples 1 to 5 are shown in table 1:
TABLE 1 analysis of nuclear pure beryllium oxide samples
As can be seen from Table 1, the method for preparing high-purity beryllium oxide by using the method of dissolving beryllium oxide in high-concentration alkali liquor, purifying beryllium hydroxide by hydrolysis and closed clean calcination has the advantages of short process flow, low production cost and strong adaptability to raw materials. The beryllium oxide prepared in the embodiments 1-5 has high main content, 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 hydroxide is characterized by comprising the following steps:
1) dissolving industrial-grade beryllium oxide in a sodium hydroxide solution;
2) adding the dissolved solution into pure water to perform hydrolysis reaction;
3) after the reaction is finished, performing centrifugal separation, wherein the solid beryllium hydroxide is washed and dried by pure water to obtain high-purity beryllium hydroxide; and (3) evaporating and concentrating the separated liquid, and circularly dissolving the industrial-grade beryllium oxide in the step 1).
2. The method for preparing high-purity beryllium hydroxide according to claim 1, wherein the temperature of the dissolution process in the step 1) is 120 to 200 ℃.
3. The method for preparing high-purity beryllium hydroxide according to claim 1, wherein in the step 1), the molar ratio of sodium hydroxide to industrial-grade beryllium oxide is (2-8): 1.
4. The method for preparing high-purity beryllium hydroxide according to claim 1, wherein the mass fraction of sodium hydroxide in the step 1) is 60 to 90%.
5. The method for producing high-purity beryllium hydroxide according to claim 1, wherein the hydrolysis reaction temperature in the step 2) is 25 to 90 ℃.
6. The method for producing high-purity beryllium hydroxide according to claim 1, wherein the volume ratio of pure water to the dissolving solution in the step 2) is (10-20): 1.
7. The method for preparing high-purity beryllium hydroxide according to claim 1, wherein in the step 3), the mass ratio of pure water to solid beryllium hydroxide in the washing process is (8-16): 1, the washing time is 1-3 h, the temperature in the drying process is 70-150 ℃, and the drying time is 2-6 h.
8. The method for preparing high-purity beryllium hydroxide according to claim 1, wherein in the step 3), the mass fraction of the solute of the separation solution after evaporation and concentration is 60-90%.
9. A method for preparing nuclear pure beryllium oxide, which is characterized in that the high-purity beryllium hydroxide in any one of claims 1 to 8 is calcined in a clean calcination-high-temperature beryllium dust recovery system which is closed in the whole process.
10. The preparation method according to claim 9, wherein the calcining temperature is 900-1200 ℃, the calcining time is 8-15 h, and the part of the contact material of the calcining furnace is made of high-purity quartz or high-purity corundum material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114538896A (en) * | 2022-01-28 | 2022-05-27 | 中国科学院近代物理研究所 | Method for producing beryllium oxide ceramic balls in large scale by adopting roll forming process |
| CN114671444A (en) * | 2022-04-08 | 2022-06-28 | 上海太洋科技有限公司 | Beryllium oxide and preparation method thereof |
| CN115340111A (en) * | 2022-08-30 | 2022-11-15 | 峨眉山市中山新材料科技有限公司 | Preparation process and product of industrial beryllium oxide capable of recycling beryllium-containing components in cleaning solution |
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| CN105585034A (en) * | 2016-01-13 | 2016-05-18 | 南华大学 | Method for preparing high-purity beryllium hydroxide from low-purity beryllium hydroxide |
| CN108950181A (en) * | 2018-07-04 | 2018-12-07 | 峨眉山市中山新材料科技有限公司 | A kind of preparation process of beryllium oxide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103663506A (en) * | 2013-12-06 | 2014-03-26 | 富蕴恒盛铍业有限责任公司 | Preparation method for refined beryllium hydroxide and preparation method for reactor-quality metallic beryllium bead from refined beryllium hydroxide |
| CN105585034A (en) * | 2016-01-13 | 2016-05-18 | 南华大学 | Method for preparing high-purity beryllium hydroxide from low-purity beryllium hydroxide |
| CN108950181A (en) * | 2018-07-04 | 2018-12-07 | 峨眉山市中山新材料科技有限公司 | A kind of preparation process of beryllium oxide |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538896A (en) * | 2022-01-28 | 2022-05-27 | 中国科学院近代物理研究所 | Method for producing beryllium oxide ceramic balls in large scale by adopting roll forming process |
| CN114671444A (en) * | 2022-04-08 | 2022-06-28 | 上海太洋科技有限公司 | Beryllium oxide and preparation method thereof |
| CN114671444B (en) * | 2022-04-08 | 2023-11-07 | 上海太洋科技有限公司 | Beryllium oxide and preparation method thereof |
| CN115340111A (en) * | 2022-08-30 | 2022-11-15 | 峨眉山市中山新材料科技有限公司 | Preparation process and product of industrial beryllium oxide capable of recycling beryllium-containing components in cleaning solution |
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