Method for purifying and removing impurities from metallic rubidium cesium

Abstract

The application relates to a purification method for purifying and removing impurities of metal rubidium and cesium, which is realized by external element purification and removal of impurities, and is characterized by the following process steps and conditions: (1) first, metal lead particles are placed in a porous and liftable stainless steel net, then a vacuum-sealed Westlin bottle containing primary metal rubidium / cesium liquid is transferred into an argon-protected glove box, the Westlin bottle cover is opened, the primary metal rubidium / cesium liquid is transferred into a reaction tank, then the reaction tank and the stainless steel net are placed into a well-type resistance vacuum furnace to complete the furnace loading operation; (2) the reaction tank after the furnace loading operation is heated by a resistance heater, the furnace temperature is raised to 50-320 DEG C, after 2-10 h of heat preservation, solid-liquid separation is carried out to obtain high-purity metal rubidium / cesium, the Li / Na impurities can be effectively removed, high-purity metal rubidium / cesium products are prepared, and the method has the advantages of short process flow, low energy consumption, low reaction temperature, simple equipment operation, low cost, large or small specification, low investment, reduced environmental pollution, reduced raw material cost and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of non-ferrous metal purification, and particularly relates to a purification method for purifying and removing impurities from metal rubidium and cesium. BACKGROUND

[0002] Rubidium / cesium has unique physical and chemical properties, and high-purity metal rubidium / cesium is an important metal material for national defense technology, space industry and military high-tech equipment in China. Rubidium / cesium metal is irreplaceable in many industries, and the current main application fields include atomic clocks, ion engines, lasers, energy fields, chemical fields, medical fields and the like. With the continuous progress of science and technology, the quality requirements of metal rubidium / cesium for various applications are also continuously improved, and the preparation of high-purity rubidium / cesium products has always been a research hotspot. The preparation methods of metal rubidium / cesium are roughly divided into electrolysis method, thermal decomposition method and metal thermal reduction method, and the prepared products usually have a purity of 99.5% for rubidium and 99.9% for cesium. In order to prepare metal rubidium / cesium with higher purity, repeated distillation is adopted, which has the problems of single treatment means, easy introduction of external impurities in the repeated distillation process, unobvious impurity removal effect, low yield and high cost.

[0003] Therefore, it is of great significance to develop a purification method for purifying and removing impurities from metal rubidium and cesium by introducing external elements. SUMMARY

[0004] The present application relates to the technical field of non-ferrous metal purification, and particularly relates to a purification method for purifying and removing impurities from metal rubidium and cesium.

[0005] The principle of the present application is that metal lead is used as a purification medium and mixed with primary metal rubidium / cesium to occur solid solution reaction at a temperature not exceeding the melting point of metal lead. The purification medium can form a solid solution with impurity metals Na / Li in the primary metal rubidium / cesium. According to the difference in melting points between the solid solution and the metal rubidium / cesium, a certain temperature is maintained to make the two exist in solid-liquid two phases. Finally, high-purity metal rubidium / cesium is obtained by solid-liquid separation, and the impurities Na / Li in the primary metal rubidium / cesium are purified.

[0006] Basic knowledge: the melting point of metal cesium is 28.5℃; the melting point of metal rubidium is 39.5℃; and the melting point of metal lead is 327.46℃.

[0007] Experiments show that at a temperature of 320℃, the solid solution mass fractions of impurity elements Li and Na in the metal lead in the metal rubidium / cesium melt are 2.5wt.% and 12wt.% respectively, and the metal Rb / Cs has no solid solubility in the metal lead.

[0008] The task of the present application is accomplished by the following technical scheme:

[0009] The purification method of the metal rubidium and cesium purification and impurity removal is to remove impurities by introducing external elements, and the purification and impurity removal treatment is performed on the metal rubidium and cesium, and specifically includes the following process steps and conditions:

[0010] (1) First, the metal lead particles are placed in a porous and liftable stainless steel mesh, and then the vacuum-sealed primary metal rubidium / cesium liquid in a test tube is transferred to an argon-protected glove box, the test tube cap is opened, the primary metal rubidium / cesium liquid is transferred to a reaction tank, and then the reaction tank and the stainless steel mesh are placed in a well-type resistance vacuum furnace to complete the furnace loading operation;

[0011] (2) The reaction tank after the furnace loading operation is heated by a resistance heater, the furnace temperature is raised to 50-320 DEG C, and after 2-10 h of heat preservation, solid-liquid separation is performed to obtain high-purity metal rubidium / cesium.

[0012] Compared with the prior art, the present application has the following advantages or effects:

[0013] Because the metal lead is used as the purification medium, the Li / Na impurities can be effectively removed, the high-purity metal rubidium / cesium product is prepared, and the process flow is short and the energy consumption is low; at the same time, since only a common resistance heater is used for heating and temperature control, the reaction temperature is low; in addition, since the main equipment, the well-type vacuum resistance furnace, is a conventional furnace, the equipment operation is simple, the cost is relatively low, the specification can be large or small, and the investment is saved; in addition, since the purification medium, the metal lead, can be recycled in multiple production processes, environmental pollution can be reduced, and the raw material cost can be reduced.

[0014] The % in the application file is the mass percentage. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a schematic diagram of the purification method of the metal rubidium and cesium purification and impurity removal according to the present application.

[0016] The present application will be further described in detail below in combination with the drawings. DETAILED DESCRIPTION

[0017] As Figure 1 shown, the purification method of the metal rubidium and cesium purification and impurity removal is to remove impurities by introducing external elements, and the purification and impurity removal treatment is performed on the metal rubidium and cesium, and specifically includes the following process steps and conditions:

[0018] (1) first, the metal lead particles are placed in a porous and liftable stainless steel mesh, second, the erlenmeyer flask with primary metal rubidium / cesium liquid in vacuum sealing is transferred to the argon-protected glove box, the erlenmeyer flask cover is opened to transfer the primary metal rubidium / cesium liquid to the reaction tank, and then the reaction tank and the stainless steel mesh are placed in the well-type resistance vacuum furnace to complete the furnace loading operation;

[0019] (2) the reaction tank after the furnace loading operation is heated by a resistance heater, the furnace temperature is raised to 50-320℃, and after 2-10h of heat preservation, solid-liquid separation can obtain high-purity metal rubidium / cesium.

[0020] The purification method for purifying and removing impurities of metal rubidium and cesium of the present application is further:

[0021] The average particle size of the metal lead particles in the step (1) is limited to 1-5mm, and the purity is ≥99.99%.

[0022] The purity of the primary metal rubidium in the step S1 is 99.50-99.70%, and the purity of the cesium metal is 99.950-99.970%.

[0023] The argon gas in the glove box in the step (1) has a purity of ≥99.999%.

[0024] The reaction tank in the step (1) is cleaned with 3-5% hydrochloric acid and deionized water in sequence before use, and then rinsed with ethanol and dried.

[0025] The weight ratio of the primary metal rubidium / cesium to the metal lead particles in the step (1) is 2:1-5:1.

[0026] The solid-liquid separation in the step (2) is that the metal lead particles are placed in a porous and liftable stainless steel mesh, the metal rubidium / cesium is placed in the reaction tank, and then the reaction tank and the stainless steel mesh are placed in the well-type vacuum resistance furnace, the temperature is raised to the set temperature and then heat preserved, after the heat preservation is completed, the stainless steel mesh is lifted to separate the two materials, the high-purity metal rubidium / cesium is obtained in the crucible, the purity of the high-purity metal rubidium reaches 99.95%, the purity of the high-purity metal rubidium and cesium reaches 99.995%, and the alloyed metal lead is obtained in the stainless steel mesh.

[0027] The metal lead particles in the step (1) can be recycled in multiple production processes.

[0028] The resistance heater in the step (2) is a common heating temperature control device with low reaction temperature.

[0029] The well-type vacuum resistance furnace in the step (1) is a conventional vacuum resistance furnace.

[0030] The impurity elements in the metal rubidium to be purified in this embodiment include Li, Na and the like, wherein the mass percentage content of Li is 82x10-4%, and the mass percentage content of Na is 78x10-4%.

[0031] The method for purifying the metal rubidium in this embodiment includes the following steps.

[0032] (1) The reaction tank is sequentially cleaned with 3-5% hydrochloric acid and deionized water before use, and then rinsed with ethanol and dried.

[0033] (2) 50g of metal lead particles (average particle size 1mm, purity 99.99%) are placed in a porous and liftable stainless steel mesh, and then a vacuum-sealed vial containing 100g of primary metal rubidium liquid (purity 99.50%) is transferred into a glove box protected by argon (purity 99.999%), the vial cap is opened, the primary metal rubidium liquid is transferred into the reaction tank, and then the reaction tank and the stainless steel mesh are placed in a pit-type resistance vacuum furnace, the heating system is started, the temperature is raised to 300°C, and the temperature is kept for 4h. After the temperature keeping is completed, the two materials are separated by the lifting device, and after the lifting is completed, the temperature is lowered to room temperature, the materials are taken out, high-purity rubidium is obtained in the reaction tank, and alloyed lead is obtained in the porous stainless steel mesh.

[0034] (3) The valve of the reaction tank is closed, the reaction tank is taken out of the glove box, and then the reaction tank is heated and melted again in the glove box for sub-packaging and sampling analysis.

[0035] As shown in Table 1, the impurity content table of the high-purity metal rubidium collected in the reaction tank after the above process is as follows:

[0036]

[0037] Example 2

[0038] The impurity elements in the metal rubidium to be purified in this embodiment include Li, Na and the like, wherein the mass percentage content of Li is 91x10-4%, and the mass percentage content of Na is 63x10-4%.

[0039] The method for purifying the metal rubidium in this embodiment includes the following steps.

[0040] (1) The reaction tank is sequentially cleaned with 3-5% hydrochloric acid and deionized water before use, and then rinsed with ethanol and dried.

[0041] (2) Take the metal lead particles (average particle size 5 mm, purity of 99.99%) material 50 g in the porous and can be lifted stainless steel net, second, vacuum sealed with 100 g of primary metal rubidium (purity of 99.50%) liquid in the erlenmeyer flask, transferred to the argon (purity of 99.999%) protective glove box, open the erlenmeyer flask cap and transfer the primary metal rubidium liquid to the reaction tank, then put the reaction tank and stainless steel net into the well type resistance vacuum furnace, start the heating system, heat to 200℃, the holding time is 4h, after holding, separate the two materials by lifting device, after lifting, cool to room temperature, take out the material, get high purity rubidium in the reaction tank, and get alloyed lead in the porous stainless steel net.

[0042] (3) Close the valve of the reaction tank, take out the reaction tank and then melt again in the glove box for sub-packaging and sampling analysis.

[0043] As shown in Table 2, for the batch of primary metal rubidium raw material, the impurity content of high purity metal rubidium collected in the reaction tank after the above process is shown in the following table:

[0044]

[0045] Example 3

[0046] The impurity elements in the metal rubidium to be purified in this example include Li, Na and other elements, wherein the mass percentage of Li is 93x10-4%, and the mass percentage of Na is 69x10-4%.

[0047] The method for purifying metal rubidium in this example includes the following steps.

[0048] (1) The reaction tank is cleaned with 3-5% hydrochloric acid and deionized water before use, and then rinsed with ethanol and dried.

[0049] (2) Take the metal lead particles (average particle size 3 mm, purity of 99.99%) material 50 g in the porous and can be lifted stainless steel net, second, vacuum sealed with 150 g of primary metal rubidium (purity of 99.70%) liquid in the erlenmeyer flask, transferred to the argon (purity of 99.999%) protective glove box, open the erlenmeyer flask cap and transfer the primary metal rubidium liquid to the reaction tank, then put the reaction tank and stainless steel net into the well type resistance vacuum furnace, start the heating system, heat to 250℃, the holding time is 4h, after holding, separate the two materials by lifting device, after lifting, cool to room temperature, take out the material, get high purity rubidium in the reaction tank, and get alloyed lead in the porous stainless steel net.

[0050] (3) Close the valve of the reaction tank, take out the reaction tank and then melt again in the glove box for sub-packaging and sampling analysis.

[0051] The impurity content of the high-purity cesium collected in the reaction tank after the above process is shown in Table 4:

[0052]

[0053] Example 4

[0054] The impurity elements in the cesium to be purified in this example include Li, Na, etc., wherein the mass percentage of Li is 88x10-4%, and the mass percentage of Na is 71x10-4%.

[0055] The method for purifying cesium in this example includes the following steps.

[0056] (1) The reaction tank is cleaned with 3-5% hydrochloric acid and deionized water before use, and then rinsed with ethanol and dried.

[0057] (2) 50g of lead particles (average particle size 3mm, purity 99.99%) are placed in a porous and liftable stainless steel mesh, and then a vacuum-sealed vial containing 200g of primary cesium (purity 99.950%) is transferred to a glove box protected by argon (purity 99.999%), the vial cap is opened, and the primary cesium liquid is transferred to the reaction tank, then the reaction tank and the stainless steel mesh are placed in a pit-type resistance vacuum furnace, the heating system is started, the temperature is raised to 150°C, and the temperature is maintained for 8h, after the temperature maintaining is completed, the two materials are separated by the lifting device, after the lifting is completed, the temperature is lowered to room temperature, the materials are taken out, and high-purity cesium is obtained in the reaction tank, and alloyed lead is obtained in the porous stainless steel mesh.

[0058] (3) The valve of the reaction tank is closed, the reaction tank is removed from the glove box, and then re-melted and packaged in the glove box for sampling and analysis.

[0059] The impurity content of the high-purity cesium collected in the reaction tank after the above process is shown in Table 4:

[0060]

[0061] Example 5

[0062] The impurity elements in the cesium to be purified in this example include Li, Na, etc., wherein the mass percentage of Li is 96x10-4%, and the mass percentage of Na is 80x10-4%.

[0063] The method for purifying cesium in this example includes the following steps.

[0064] (1) The reaction tank is cleaned with 3-5% hydrochloric acid and deionized water in sequence before use, and then washed with ethanol and dried.

[0065] (2) 50g of metal lead particles (average particle size 2mm, purity 99.99%) were placed in a porous and liftable stainless steel mesh. Then, a vacuum-sealed vial containing 150g of primary cesium metal liquid (purity 99.960%) was transferred to an argon (purity 99.999%) protected glove box, the vial cap was opened, and the primary cesium metal liquid was transferred to the reaction tank. Then, the reaction tank and the stainless steel mesh were placed in an electric resistance vacuum furnace, the heating system was started, and the temperature was raised to 300°C. The temperature was maintained for 6h. After the temperature maintenance was completed, the two materials were separated by the lifting device. After the lifting was completed, the temperature was lowered to room temperature, the materials were taken out, and high-purity cesium was obtained in the reaction tank, and alloyed lead was obtained in the porous stainless steel mesh.

[0066] (3) The valve of the reaction tank was closed, and the reaction tank was removed from the glove box for hot melting, dispensing, and sampling analysis.

[0067] As shown in Table 5, the impurity content of the high-purity cesium collected in the reaction tank after the above process was as follows:

[0068]

[0069] Example 6

[0070] The impurity elements in the cesium metal to be purified in this example include Li, Na, and the like, wherein the mass percentage of Li is 82x10-4%, and the mass percentage of Na is 94x10-4%.

[0071] The method for purifying cesium metal in this example includes the following steps.

[0072] (1) The reaction tank is cleaned with 3-5% hydrochloric acid and deionized water in sequence before use, and then washed with ethanol and dried.

[0073] (2) 50g of metal lead particles (average particle size 2mm, purity 99.99%) were placed in a porous and liftable stainless steel mesh. Then, a vacuum-sealed vial containing 150g of primary cesium metal liquid (purity 99.960%) was transferred to an argon (purity 99.999%) protected glove box, the vial cap was opened, and the primary cesium metal liquid was transferred to the reaction tank. Then, the reaction tank and the stainless steel mesh were placed in an electric resistance vacuum furnace, the heating system was started, and the temperature was raised to 300°C. The temperature was maintained for 6h. After the temperature maintenance was completed, the two materials were separated by the lifting device. After the lifting was completed, the temperature was lowered to room temperature, the materials were taken out, and high-purity cesium was obtained in the reaction tank, and alloyed lead was obtained in the porous stainless steel mesh.

[0074] (3) Close the valve of the reactor, remove the reactor and then melt it again in the glove box to perform the sub-packaging and sampling analysis.

[0075] As shown in Table 6, the impurity content table of the high-purity cesium metal collected in the reactor after the above process for the batch of primary cesium metal raw material is as follows:

[0076]

[0077] As described above, the present application can be better implemented. The above examples are only the best embodiments of the present application, but the embodiments of the present application are not limited by the above examples, and other changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present application should be equivalent replacement methods, and all are included in the protection scope of the present application.

Claims

1. A method for purifying and removing impurities from metallic rubidium and cesium, characterized in that The metal rubidium and cesium are purified and impurity-removed by introducing external elements, which specifically includes the following process steps and conditions: (1) First, place the lead pellets in a porous and elevatable stainless steel mesh. Then, transfer the vacuum-sealed vial containing the primary metal rubidium / cesium liquid to an argon-protected glove box. Open the vial cap and transfer the primary metal rubidium / cesium liquid to the reaction tank. Then, place the reaction tank and the stainless steel mesh together in a well-type resistance vacuum furnace to complete the furnace loading operation. (2) The reaction tank after the furnace loading operation is heated with a resistance heater to raise the furnace temperature to 150-320°C. After keeping the temperature for 2-10 hours, the stainless steel mesh is lifted to separate the two materials, and high-purity metallic rubidium / cesium is obtained in the reaction tank, and alloyed metallic lead is obtained in the stainless steel mesh.

2. The method according to claim 1, wherein The average particle size of the lead metal particles introduced in step (1) is limited to 1-5 mm, and the purity is ≥99.99 wt%.

3. The method according to claim 1, wherein In the step (1), the purity of the primary metallic rubidium is 99.50-99.70 wt%, and the purity of the primary metallic cesium is 99.950-99.970 wt%.

4. The method according to claim 1, wherein The purity of the argon gas in the glove box in step (1) is ≥99.999 wt%.

5. The method according to claim 1, wherein The reaction tank in step (1) is cleaned with 3-5 wt% hydrochloric acid and deionized water in sequence before use, and then rinsed with ethanol and dried.

6. The method according to claim 1, 2, 3, 4 or 5, wherein In the step (1), the weight ratio of the primary metal rubidium / cesium to the metal lead particles is 2:1 to 5:

1.

7. The method according to claim 1 or 2, wherein The purity of the high-purity cesium metal reaches 99.995wt%, and the purity of the high-purity rubidium metal reaches 99.95wt%.

8. The method according to claim 1, wherein The metal lead particles in step (1) are recycled in multiple production processes.

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