Purification method for purification and impurity removal of metal rubidium and cesium

Abstract

A purification method for purification and impurity removal of metal rubidium and cesium performs purification and impurity removal treatment on metal rubidium and cesium through external introduction of elements, and specifically comprises the following process steps and conditions: (1) firstly, putting metal lead particles into a porous and liftable stainless steel mesh; secondly, transferring a penicillin bottle in which the primary metal rubidium / cesium liquid is sealed in a vacuum manner into a glove box protected by argon, opening a penicillin bottle cap to transfer the primary metal rubidium / cesium liquid into a reaction tank, and then putting the reaction tank and a stainless steel mesh into a well type resistance vacuum furnace together to finish charging operation; and (2) heating the reaction tank after the charging operation by using a resistance heater, raising the temperature of the furnace to 50-320 DEG C, keeping the temperature for 2-10 hours, and then carrying out solid-liquid separation to obtain the high-purity metal rubidium / cesium, so that Li / Na impurities can be effectively removed, a high-purity metal rubidium / cesium product is prepared, and the production cost is reduced. And the method has the advantages of short process flow, low energy consumption, low reaction temperature, simplicity and convenience in equipment operation, lower manufacturing cost, variable specification, investment saving, environmental pollution reduction, raw material cost reduction and the like.

Description

Technical Field

[0001] The invention relates to the technical field of nonferrous metal purification, and in particular to a purification method for purifying and removing impurities from metal rubidium and cesium. Background Art

[0002] Rubidium / cesium has unique physical and chemical properties. High-purity metallic rubidium / cesium is an important metal material for my country's national defense technology, aerospace industry and military high-tech equipment. Rubidium / cesium metal is irreplaceable in many industries. At present, its main application areas include atomic clocks, ion engines, lasers, energy fields, chemical fields, medical fields, etc. With the continuous advancement of science and technology, the quality requirements of metallic rubidium / cesium for various applications are also constantly increasing. The preparation of high-purity rubidium / cesium products has always been a research hotspot. The preparation methods of metallic rubidium / cesium are roughly divided into electrolysis, thermal decomposition and metal thermal reduction. The purity of the prepared products is usually 99.5% for rubidium and 99.9% for cesium. If you want to prepare metallic rubidium / cesium with higher purity, you need to use repeated distillation. There are problems such as single treatment means and repeated distillation process, which is easy to introduce external impurities, poor effect, low yield and high cost.

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

[0004] The task of the present invention is to overcome the shortcomings of the prior art and provide a purification method for purifying and removing impurities from metallic rubidium and cesium. By introducing external elements, it can not only solve the problems of low efficiency and unclear impurity removal effect of traditional distillation, but also produce high-purity metallic rubidium / cesium products.

[0005] The principle of the present invention is: metal lead is used as a purification medium, mixed with primary metal rubidium / cesium, and a solid solution reaction occurs at a temperature not exceeding the melting point of the metal lead. The purification medium can form a solid solution with the impurity metal 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 so that the two exist in solid-liquid two phases. Finally, high-purity metal rubidium / cesium is obtained by solid-liquid separation, thereby achieving purification of the impurity Na / Li in the primary metal rubidium / cesium.

[0006] Basic knowledge: The melting point of metallic cesium is 28.5°C; the melting point of metallic rubidium is 39.5°C; the melting point of metallic lead is 327.46°C.

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

[0008] The task of the present invention is accomplished by the following technical solutions:

[0009] The purification method of rubidium and cesium metals by purifying and removing impurities through external element purification and impurities removal, specifically includes the following process steps and conditions:

[0010] (1) First, place the metal lead pellets in a porous and liftable 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 a reaction tank, then place the reaction tank and the stainless steel mesh together in a pit-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 to raise the furnace temperature to 50-320° C., and after keeping the temperature for 2-10 hours, high-purity metallic rubidium / cesium can be obtained by solid-liquid separation.

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

[0013] Because metal lead is used as the purification medium, Li / Na impurities can be effectively removed to produce high-purity metal rubidium / cesium products, and the process flow is short and the energy consumption is low. At the same time, because only ordinary resistance heaters are needed for heating and temperature control, the reaction temperature is low. In addition, because the main equipment, the pit-type vacuum resistance furnace, is a conventional furnace, the equipment is easy to operate, the cost is low, the specifications can be large or small, and the investment is low. In addition, because the purification medium metal lead can be recycled in multiple production processes, it can reduce environmental pollution and reduce raw material costs.

[0014] The % mentioned in the application documents refers to mass percentage. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of a purification method for purifying and removing impurities from metallic rubidium and cesium proposed in the present invention.

[0016] The present invention is further described in detail below in conjunction with the accompanying drawings. DETAILED DESCRIPTION

[0017] like Figure 1 As shown, the purification method for purifying and removing impurities of metallic rubidium and cesium is aimed at the problems that the existing technology has a single treatment method and the repeated distillation process is easy to introduce external impurities, the effect is not obvious, the yield is low and the cost is high. It is characterized by purifying and removing impurities by introducing external elements, and purifying and removing impurities for metallic rubidium and cesium, and specifically includes the following process steps and conditions:

[0018] (1) First, place the metal lead pellets in a porous and liftable 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 a reaction tank, then place the reaction tank and the stainless steel mesh together in a pit-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 to raise the furnace temperature to 50-320° C., and after keeping the temperature for 2-10 hours, high-purity metallic rubidium / cesium can be obtained by solid-liquid separation.

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

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

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

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

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

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

[0026] The solid-liquid separation in step (2) is to place the metal lead particles in a porous and liftable stainless steel mesh, place the metal rubidium / cesium in a reaction tank, then place the reaction tank and the stainless steel mesh together in a pit-type vacuum resistance furnace, heat them to a set temperature and then keep them warm, and after the insulation is completed, lift the stainless steel mesh to separate the two materials, and obtain high-purity metal rubidium / cesium in the crucible, the purity of the high-purity metal rubidium reaches 99.95%, and the purity of the high-purity metal rubidium and cesium reaches 99.995%, and alloyed metal lead is obtained in the stainless steel mesh.

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

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

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

[0030] The impurity elements in the metallic rubidium to be purified in this embodiment include elements such as Li and Na, wherein the mass percentage of Li is 82×10-4%, and the mass percentage of Na is 78×10-4%.

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

[0032] (1) Before use, the reaction tank was cleaned with 3-5% hydrochloric acid and deionized water, rinsed with ethanol and then dried.

[0033] (2) Take 50 g of metal lead particles (average particle size 1 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 100 g of primary metal rubidium (purity 99.50%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metal rubidium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 300°C, and keep the temperature for 4 hours. After the insulation is completed, separate the two materials through a lifting device. After the lifting is completed, cool to room temperature, take out the materials, obtain high-purity rubidium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0034] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

[0035] As shown in Table 1, this is the impurity content of the high-purity rubidium metal collected in the reaction tank after the above process for this batch of primary rubidium metal raw materials:

[0036]

[0037] Example 2

[0038] The impurity elements in the metallic rubidium to be purified in this embodiment include elements such as Li and Na, wherein the mass percentage of Li is 91×10-4%, and the mass percentage of Na is 63×10-4%.

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

[0040] (1) Before use, the reaction tank was cleaned with 3-5% hydrochloric acid and deionized water, rinsed with ethanol and then dried.

[0041] (2) Take 50 g of metal lead particles (average particle size 5 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 100 g of primary metal rubidium (purity 99.50%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metal rubidium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 200°C, and keep the temperature for 4 hours. After the end of the insulation, separate the two materials through a lifting device. After the end of the lifting, cool to room temperature, take out the materials, obtain high-purity rubidium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0042] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

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

[0044]

[0045] Example 3

[0046] The impurity elements in the metallic rubidium to be purified in this embodiment include elements such as Li and Na, wherein the mass percentage of Li is 93×10-4%, and the mass percentage of Na is 69×10-4%.

[0047] The method for purifying metallic rubidium in this embodiment includes the following steps.

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

[0049] (2) Take 50 g of metal lead particles (average particle size 3 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 150 g of primary metal rubidium (purity 99.70%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metal rubidium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 250°C, and keep the temperature for 4 hours. After the insulation is completed, separate the two materials through a lifting device. After the lifting is completed, cool to room temperature, take out the materials, obtain high-purity rubidium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0050] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

[0051] As shown in Table 3, this is the impurity content of the high-purity rubidium metal collected in the reaction tank after the above process for this batch of primary rubidium metal raw materials:

[0052]

[0053] Example 4

[0054] The impurity elements in the metallic cesium to be purified in this embodiment include Li, Na and other elements, wherein the mass percentage of Li is 88×10-4%, and the mass percentage of Na is 71×10-4%.

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

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

[0057] (2) Take 50 g of metal lead particles (average particle size 3 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 200 g of primary metallic cesium (purity 99.950%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metallic cesium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 150°C, and keep the temperature for 8 hours. After the insulation is completed, separate the two materials through a lifting device. After the lifting is completed, cool the temperature to room temperature, take out the materials, obtain high-purity cesium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0058] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

[0059] As shown in Table 4, this is the impurity content of the high-purity cesium metal collected in the reaction tank after the above process for the batch of primary cesium metal raw materials:

[0060]

[0061] Example 5

[0062] The impurity elements in the metallic cesium to be purified in this embodiment include elements such as Li and Na, wherein the mass percentage of Li is 96×10-4%, and the mass percentage of Na is 80×10-4%.

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

[0064] (1) Before use, the reaction tank was cleaned with 3-5% hydrochloric acid and deionized water, rinsed with ethanol and then dried.

[0065] (2) Take 50 g of metal lead particles (average particle size 2 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 150 g of primary metallic cesium (purity 99.960%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metallic cesium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 300°C, and keep the temperature for 6 hours. After the end of the insulation, separate the two materials through a lifting device. After the end of the lifting, cool the temperature to room temperature, take out the materials, obtain high-purity cesium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0066] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

[0067] As shown in Table 5, this is the impurity content of the high-purity cesium metal collected in the reaction tank after the above process for this batch of primary cesium metal raw materials:

[0068]

[0069] Example 6

[0070] The impurity elements in the metallic cesium to be purified in this embodiment include elements such as Li and Na, wherein the mass percentage of Li is 82×10-4%, and the mass percentage of Na is 94×10-4%.

[0071] The method for purifying metallic cesium in this embodiment includes the following steps.

[0072] (1) Before use, the reaction tank was cleaned with 3-5% hydrochloric acid and deionized water, rinsed with ethanol and then dried.

[0073] (2) Take 50 g of metal lead particles (average particle size 1 mm, purity 99.99%) and place them in a porous and liftable stainless steel mesh. Then, transfer a vacuum-sealed vial containing 150 g of primary metallic cesium (purity 99.950%) liquid to a glove box protected by argon (purity 99.999%). Open the vial cap and transfer the primary metallic cesium liquid to a reaction tank. Then, place the reaction tank and the stainless steel mesh together in a pit-type resistance vacuum furnace, start the heating system, raise the temperature to 250°C, and keep the temperature for 6 hours. After the end of the heat preservation, separate the two materials through a lifting device. After the end of the lifting, cool the temperature to room temperature, take out the materials, obtain high-purity cesium in the reaction tank, and obtain alloyed lead in the porous stainless steel mesh.

[0074] (3) Close the valve of the reaction tank, remove the reaction tank, and then heat-melt it again in the glove box for subpackaging and sampling analysis.

[0075] As shown in Table 6, this is the impurity content of the high-purity cesium metal collected in the reaction tank after the above process for this batch of primary cesium metal raw materials:

[0076]

[0077] As described above, the present invention can be better implemented. The above embodiments are only the best implementation methods of the present invention, but the implementation methods of the present invention are not limited by the above embodiments. Other changes, modifications, replacements, combinations, and simplifications made without departing from the spirit and principle of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A purification method for purifying and removing impurities from metallic rubidium and cesium, which aims to solve the problems of the prior art that the treatment means are single and the repeated distillation process easily introduces external impurities, the effect is not obvious, the yield is low and the cost is high. It is characterized by The metal rubidium and cesium are purified and impurity-removed by external element purification and impurity removal, which specifically includes the following process steps and conditions: (1) First, place the metal lead pellets in a porous and liftable 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 a reaction tank, then place the reaction tank and the stainless steel mesh together in a pit-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 to raise the furnace temperature to 50-320° C., and after keeping the temperature for 2-10 hours, high-purity metallic rubidium / cesium can be obtained by solid-liquid separation.

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

3. The method according to claim 1, characterized in that In step S1, the purity of primary rubidium metal is 99.50-99.70%, and the purity of cesium metal is 99.950-99.970%.

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

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

6. The method according to claim 1 or 2 or 3 or 4 or 5, characterized in that 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, characterized in that The solid-liquid separation in step (2) is to place the metal lead particles in a porous and liftable stainless steel mesh, place the metal rubidium / cesium in a reaction tank, then place the reaction tank and the stainless steel mesh together in a pit-type vacuum resistance furnace, heat them to a set temperature and then keep them warm, and after the insulation is completed, lift the stainless steel mesh to separate the two materials, and obtain high-purity metal rubidium / cesium in the crucible, the purity of the high-purity metal rubidium reaches 99.95%, and the purity of the high-purity metal rubidium and cesium reaches 99.995%, and alloyed metal lead is obtained in the stainless steel mesh.

8. The method according to claim 1, characterized in that The metal lead particles in step (1) can be recycled in multiple production processes.

9. The method according to claim 1, characterized in that The resistance heater in step (2) is a common heating and temperature control device with a low reaction temperature.

10. The method according to claim 1, characterized in that The pit-type vacuum resistance furnace in step (1) is a conventional vacuum resistance furnace.

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