CN113735144A - Preparation method of high-purity anhydrous rubidium iodide - Google Patents
Preparation method of high-purity anhydrous rubidium iodide Download PDFInfo
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- CN113735144A CN113735144A CN202111079585.7A CN202111079585A CN113735144A CN 113735144 A CN113735144 A CN 113735144A CN 202111079585 A CN202111079585 A CN 202111079585A CN 113735144 A CN113735144 A CN 113735144A
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- WFUBYPSJBBQSOU-UHFFFAOYSA-M rubidium iodide Chemical compound [Rb+].[I-] WFUBYPSJBBQSOU-UHFFFAOYSA-M 0.000 title claims abstract description 208
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 53
- WPFGFHJALYCVMO-UHFFFAOYSA-L rubidium carbonate Chemical compound [Rb+].[Rb+].[O-]C([O-])=O WPFGFHJALYCVMO-UHFFFAOYSA-L 0.000 claims abstract description 44
- 229910000026 rubidium carbonate Inorganic materials 0.000 claims abstract description 44
- 239000000126 substance Substances 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012535 impurity Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 25
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 23
- 239000011630 iodine Substances 0.000 claims abstract description 23
- 238000007323 disproportionation reaction Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 17
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 10
- 238000005265 energy consumption Methods 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 5
- 238000001953 recrystallisation Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 229940071870 hydroiodic acid Drugs 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- CPRMKOQKXYSDML-UHFFFAOYSA-M rubidium hydroxide Chemical compound [OH-].[Rb+] CPRMKOQKXYSDML-UHFFFAOYSA-M 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 206010018498 Goitre Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 201000003872 goiter Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D17/00—Rubidium, caesium or francium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of high-purity anhydrous rubidium iodide. The preparation method of the high-purity anhydrous rubidium iodide comprises the following steps: step A: under the condition of normal temperature, 400-600 g of rubidium carbonate is placed into a reaction vessel, pure water with the mass liquid-solid ratio of 2-4: 1 is slowly added while stirring, and the mixture is stirred for 10-30 min until the rubidium carbonate is completely dissolved; and B: at normal temperature, filtering the solution obtained in the step A while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium carbonate solution; and C: and C, slowly pouring an iodine simple substance with the molar ratio of Li to I being 1:1 into the rubidium carbonate solution obtained in the step B under the stirring condition at normal temperature for carrying out disproportionation reaction, and stirring for 15-20 min to generate a dark brown solution. The preparation method of the high-purity anhydrous rubidium iodide has the advantages of simple and practical process, less equipment investment, low production cost, high yield, high economic value, little environmental pollution and high production safety.
Description
Technical Field
The invention relates to the technical field of solid battery electrolyte preparation, in particular to a preparation method of high-purity anhydrous rubidium iodide.
Background
Rubidium iodide has been widely used in various fields in recent years. In the medical field, rubidium iodide may sometimes replace potassium iodide in the treatment of goiter. In the field of battery materials, rubidium iodide can be used as a battery reaction material to be applied to a miniature high-energy battery; can also be used for preparing ultra-high electron conductor RbAg at room temperature4I5And is commonly used as a thin film solid battery electrolyte. In addition, in the field of photoelectric devices, a neutron detector taking the doped rubidium iodide crystal as the solid scintillator has the advantages of high light yield, large capture and volume, high detection efficiency and the like. In addition, rubidium iodide is an important chemical agent in the field of chemical organic synthesis, and is commonly used as a catalyst or an additive.
At present, the preparation method of anhydrous rubidium iodide mainly comprises a neutralization method and a pyrogenic process, wherein the neutralization method uses rubidium hydroxide as a raw material to react with hydroiodic acid, the water content of the rubidium iodide prepared by the method is higher than 200ppm, the cost of the raw material is high, and the hydroiodic acid has strong corrosivity and has strict process requirements. The pyrogenic process method is to carry out synthetic reaction on metal rubidium melted at high temperature and iodine simple substance, and high-purity anhydrous rubidium iodide can be prepared by purification. Although the water content can be below 100ppm, the method has high equipment requirement, low yield, high raw material cost and energy consumption and is difficult to realize large-scale production. The rubidium iodide obtained by the above two processes has defects, such as: the process conditions are harsh, the cost is high, and the purity is low (less than or equal to 99%).
Disclosure of Invention
In view of the above, it is necessary to provide a method for producing highly pure anhydrous rubidium iodide.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of high-purity anhydrous rubidium iodide comprises the following steps:
step A: under the condition of normal temperature, 400-600 g of rubidium carbonate is placed into a reaction vessel, pure water with the mass liquid-solid ratio of 2-4: 1 is slowly added while stirring, and the mixture is stirred for 10-30 min until the rubidium carbonate is completely dissolved;
and B: at normal temperature, filtering the solution obtained in the step A while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium carbonate solution;
and C: at normal temperature, slowly pouring an iodine simple substance with a molar ratio of Li to I of 1:1 into the rubidium carbonate solution obtained in the step B under the stirring condition for carrying out disproportionation reaction, and stirring for 15-20 min to generate a dark brown solution;
step D: at normal temperature, slowly adding 80% hydrazine hydrate by mass into the dark brown solution obtained by the reaction in the step C, controlling the addition rate of the hydrazine hydrate to be 0.3-0.5 g/s, ending the reaction when the solution is neutral and the solution is colorless and has no bubbles, and finally adding a small amount of hydrazine hydrate to ensure that the pH value of the solution is within the range of 7-9, and stirring for reaction for 1-2 hours;
step E: at normal temperature, filtering the solution with the pH of 7-9 obtained in the step D while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium iodide solution;
step F: evaporating and concentrating the rubidium iodide solution obtained in the step E under normal pressure, removing a certain amount of water, and concentrating to 105-125 ℃ to obtain rubidium iodide slurry;
step G, cooling the rubidium iodide slurry obtained in the step F to 40-50 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal;
step H, dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1: 1-2.5, filtering after the rubidium iodide crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material;
and step I, putting the wet rubidium iodide material obtained in the step H into a forced air drying oven, and drying the wet rubidium iodide material in vacuum for 2-4 hours at the temperature of 150-180 ℃ to obtain high-purity anhydrous rubidium iodide.
Furthermore, the pure water added in the step A is 2-4 times of the rubidium carbonate, a 20.0-33.3% rubidium carbonate solution is prepared, complete dissolution of the rubidium carbonate is guaranteed, the consumption of the pure water is reduced, energy consumption of subsequent evaporation concentration is reduced, and cost is saved.
Further, the dosage of the iodine simple substance in the step C is 1:1 of Rb: I molar ratio, and the iodine simple substance completely reacts for 15-20 min, which shows that the iodine particles gradually react and disappear.
Further, said hydrazine hydrate is added in excess in said step D, and a small amount of RbIO remains3The RbI is slowly reduced to make the solution alkalescent, the PH value is within the range of 7-9, and the alkaline insoluble substances can be removed during filtration, such as Ca and Fe, and the precipitation of iodine can be inhibited during the simultaneous concentration process.
Furthermore, the aperture of the sand core funnel used for filtering and removing impurities in the step B and the step E is 1-5 um, so that fine precipitates in the solution can be removed, impurities in the solution can be removed, and high-quality rubidium iodide is obtained.
And further, in the step F, under normal pressure, the temperature of a concentration end point is 105-125 ℃, the temperature of the concentration end point is too low, the free water is not completely removed, the yield after crystallization is relatively low, and if the temperature is too high, the crystal can be adhered to a container in the crystal precipitation process, so that the wall of the container is easily formed, the yield is influenced, and the container can not be used seriously.
And further, in the step G, filtering is carried out at room temperature by using a sand core funnel of 5-15 um, solid-liquid separation is carried out until no liquid seeps out, the humidity of the rubidium iodide crystal material in the funnel is ensured to be low, the carrying capacity of the attached liquid is reduced, the drying time is reduced while impurities are reduced, and the energy consumption is reduced.
And furthermore, the drying temperature in the step H is 160-170 ℃, and iodine in the product is prevented from being separated out while drying, so that the product quality is improved.
Compared with the prior art, the preparation method of high-purity anhydrous rubidium iodide can effectively solve the problems of low purity, high water content, complex synthesis process, harsh process conditions, high cost, high energy consumption, environmental pollution and the like of the existing rubidium iodide. The invention aims to solve the defects in the prior art, and aims to provide a simple and practical process with low production cost and low equipment investment, the color of the anhydrous rubidium iodide prepared by the process is white, the purities of the rubidium carbonate and iodine simple substances are more than or equal to 99 percent, the anhydrous rubidium iodide is prepared by a diamine method, the adopted reducing agent is hydrazine hydrate, the generated by-product is nitrogen, and the solution is ensured to have no redundant impurities.
The preparation method of the high-purity anhydrous rubidium iodide comprises the step of preparing a rubidium iodide solution, namely, carrying out disproportionation reaction on rubidium carbonate and iodine simple substance to generate RbI and RbIO3Then using hydrazine hydrate to react RbIO with3Reducing to RbI to obtain rubidium iodide solution. And in the second step, the concentration, crystallization and impurity removal of the rubidium iodide are carried out, namely, water in the rubidium iodide is removed by heating and concentrating to a certain temperature under normal pressure, the filtering is carried out after crystallization is separated out, then recrystallization and impurity removal are carried out, and finally drying is carried out to obtain white anhydrous rubidium iodide, wherein the water content is less than or equal to 150ppm, and the main content is more than 99.9%. In the whole process, the process is simple, the requirement on equipment is simple, the requirement on environmental conditions is loose, and the process is short. The main reaction equation is as follows: 2Rb2CO3+2I2+N2H4·H2O=4RbI+N2↑+2CO2↑+3H2O。
According to the preparation method of the high-purity anhydrous rubidium iodide, firstly, the produced product has high purity, the process flow is simple and convenient, and the preparation method is suitable for industrial production; secondly, the purity of the obtained rubidium iodide can reach more than 99.9 percent, and the moisture content is below 150 ppm; thirdly, inorganic chemical combination reaction is performed in the process of preparing the rubidium iodide, so that the conversion efficiency is high, the environment is protected, and the energy consumption and the cost are saved; finally, the processes of evaporation, concentration and recrystallization of the rubidium iodide are all carried out under atmospheric normal pressure, the reaction is stable, the requirements on process conditions are simple, the influence factors are few, and the operation is convenient.
Detailed Description
The present invention will now be described more fully hereinafter with reference to examples for the purpose of facilitating an understanding of the invention, but the invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a preparation method of high-purity anhydrous rubidium iodide, which is characterized by comprising the following steps:
step A, dissolving rubidium carbonate: under the condition of normal temperature, 400-600 g of rubidium carbonate is placed into a reaction vessel, pure water with the mass liquid-solid ratio of 2-4: 1 is slowly added while stirring, and the mixture is stirred for 10-30 min until the rubidium carbonate is completely dissolved;
and B, filtering and removing impurities: at normal temperature, filtering the solution obtained in the step A while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium carbonate solution;
step C, disproportionation reaction: at normal temperature, slowly pouring an iodine simple substance with a molar ratio of Li to I of 1:1 into the rubidium carbonate solution obtained in the step B under the stirring condition for carrying out disproportionation reaction, and stirring for 15-20 min to generate a dark brown solution;
step D, hydrazine hydrate reduction reaction: at normal temperature, slowly adding 80% hydrazine hydrate by mass into the dark brown solution obtained by the reaction in the step C, controlling the addition rate of the hydrazine hydrate to be 0.3-0.5 g/s, ending the reaction when the solution is neutral and the solution is colorless and has no bubbles, and finally adding a small amount of hydrazine hydrate to ensure that the pH value of the solution is within the range of 7-9, and stirring for reaction for 1-2 hours;
step E, filtration and impurity removal: at normal temperature, filtering the solution with the pH of 7-9 obtained in the step D while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium iodide solution;
step F, normal pressure evaporation and concentration: evaporating and concentrating the rubidium iodide solution obtained in the step E under normal pressure, removing a certain amount of water, and concentrating to 105-125 ℃ to obtain rubidium iodide slurry;
g, cooling and crystallizing, namely cooling the rubidium iodide slurry obtained in the step F to 40-50 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal;
step H, recrystallization and impurity removal, namely dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1: 1-2.5, filtering after the rubidium iodide crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material;
and step I, drying, crushing and packaging, namely putting the wet rubidium iodide material obtained in the step H into a blast drying oven, and performing vacuum drying for 2-4 hours at the temperature of 150-180 ℃ to obtain high-purity anhydrous rubidium iodide.
Furthermore, the pure water added in the step A is 2-4 times of the rubidium carbonate, a 20.0-33.3% rubidium carbonate solution is prepared, complete dissolution of the rubidium carbonate is guaranteed, the consumption of the pure water is reduced, energy consumption of subsequent evaporation concentration is reduced, and cost is saved.
Further, the dosage of the iodine simple substance in the step C is 1:1 in molar ratio of Rb to I, and the iodine simple substance completely reacts for 15-20 min, which shows that the iodine particles gradually react and disappear.
Further, said hydrazine hydrate is added in excess in said step D, and a small amount of RbIO remains3The RbI is slowly reduced to make the solution alkalescent, the PH value is within the range of 7-9, and the alkaline insoluble substances can be removed during filtration, such as Ca and Fe, and the precipitation of iodine can be inhibited during the simultaneous concentration process.
Furthermore, the aperture of the sand core funnel used for filtering and removing impurities in the step B and the step E is 2-4 um, so that fine precipitates in the solution can be removed, impurities in the solution can be removed, and high-quality rubidium iodide is obtained.
And further, in the step F, under normal pressure, the temperature of a concentration end point is 105-125 ℃, the temperature of the concentration end point is too low, the free water is not completely removed, the yield after crystallization is relatively low, and if the temperature is too high, the crystal can be adhered to a container in the crystal precipitation process, so that the wall of the container is easily formed, the yield is influenced, and the container can not be used seriously.
And further, in the step G, filtering is carried out at room temperature by using a sand core funnel of 5-15 um, solid-liquid separation is carried out until no liquid seeps out, the humidity of the rubidium iodide crystal material in the funnel is ensured to be low, the carrying capacity of the attached liquid is reduced, the drying time is reduced while impurities are reduced, and the energy consumption is reduced.
And furthermore, the drying temperature in the step H is 160-170 ℃, and iodine in the product is prevented from being separated out while drying, so that the product quality is improved.
Compared with the prior art, the preparation method of high-purity anhydrous rubidium iodide can effectively solve the problems of low purity, high water content, complex synthesis process, harsh process conditions, high cost, high energy consumption, environmental pollution and the like of the existing rubidium iodide. The invention aims to solve the defects in the prior art, and aims to provide a simple and practical process with low production cost and low equipment investment, the color of the anhydrous rubidium iodide prepared by the process is white, the purities of the rubidium carbonate and iodine simple substances are more than or equal to 99 percent, the anhydrous rubidium iodide is prepared by a diamine method, the adopted reducing agent is hydrazine hydrate, the generated by-product is nitrogen, and the solution is ensured to have no redundant impurities.
The preparation method of the high-purity anhydrous rubidium iodide comprises the step of preparing a rubidium iodide solution, namely, carrying out disproportionation reaction on rubidium carbonate and iodine simple substance to generate RbI and RbIO3Then using hydrazine hydrate to react RbIO with3Reducing to RbI to obtain rubidium iodide solution. And in the second step, the concentration, crystallization and impurity removal of the rubidium iodide are carried out, namely, water in the rubidium iodide is removed by heating and concentrating to a certain temperature under normal pressure, the filtering is carried out after crystallization is separated out, then recrystallization and impurity removal are carried out, and finally drying is carried out to obtain white anhydrous rubidium iodide, wherein the water content is less than or equal to 150ppm, and the main content is more than 99.9%. In the whole process, the process is simple, the requirement on equipment is simple, the requirement on environmental conditions is loose, and the process is short. The main reaction equation is as follows: 2Rb2CO3+2I2+N2H4·H2O=4RbI+N2↑+2CO2↑+3H2O。
According to the preparation method of the high-purity anhydrous rubidium iodide, firstly, the produced product has high purity, the process flow is simple and convenient, and the preparation method is suitable for industrial production; secondly, the purity of the obtained rubidium iodide can reach more than 99.9 percent, and the moisture content is below 150 ppm; thirdly, inorganic chemical combination reaction is performed in the process of preparing the rubidium iodide, so that the conversion efficiency is high, the environment is protected, and the energy consumption and the cost are saved; finally, the processes of evaporation, concentration and recrystallization of the rubidium iodide are all carried out under atmospheric normal pressure, the reaction is stable, the requirements on process conditions are simple, the influence factors are few, and the operation is convenient.
Example 1
Step A, dissolving rubidium carbonate: under the condition of normal temperature, 400g of rubidium carbonate is put into a reaction vessel, 800g of pure water is slowly added while stirring, and the mixture is stirred for 10min until the rubidium carbonate is completely dissolved.
And B, filtering and removing impurities: and (3) filtering the solution obtained in the step (A) at normal temperature while the solution is hot, and removing alkali insoluble substances and other impurities by using a 3-micron sand core funnel to obtain a clear and transparent rubidium carbonate solution.
Step C, disproportionation reaction: and C, slowly pouring 439.6g of iodine simple substance with the molar ratio Rb: I of 1:1 into the rubidium carbonate solution obtained in the step B under the condition of stirring at normal temperature for carrying out disproportionation reaction, and stirring for 15min to generate a dark brown solution.
Step D, hydrazine hydrate reduction reaction: and C, slowly adding 54.2g of hydrazine hydrate with the mass fraction of 80% into the dark brown solution obtained by the reaction in the step C at normal temperature, controlling the adding rate of the hydrazine hydrate to be 0.3g/s, ending the reaction when the solution is neutral and colorless and no bubbles are generated, finally adding a small amount of hydrazine hydrate to enable the pH of the solution to be 7, and stirring for reacting for 1 hour.
Step E, filtering and removing impurities: and D, filtering the solution with the pH of 7 obtained in the step D while the solution is hot at normal temperature, and removing alkali insoluble substances and other impurities by using a sand core funnel of 1um to obtain a clear and transparent rubidium iodide solution.
Step F, normal pressure evaporation and concentration: and E, evaporating and concentrating the filtered solution obtained in the step E under normal pressure to 105 ℃ to obtain rubidium iodide slurry.
Step G, cooling and crystallizing: and F, cooling the rubidium iodide slurry obtained in the step F to 40 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal.
Step H, recrystallization and impurity removal: and D, dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1:1, filtering after the rubidium carbonate crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material.
Step I, drying, crushing and packaging: and (3) putting the wet rubidium iodide material obtained in the H into a forced air drying oven, and performing vacuum drying for 4 hours at 160 ℃ to obtain the high-purity anhydrous rubidium iodide. The detection shows that the main content is 99.92 percent, and the water content is 109 ppm.
Example 2:
step A, dissolving rubidium carbonate: at normal temperature, 500g of rubidium carbonate is put into a reaction vessel, 1500g of pure water is slowly added while stirring, and stirring is carried out for 20min until the rubidium carbonate is completely dissolved.
And B, filtering and removing impurities: and (3) filtering the solution obtained in the step (A) at normal temperature while the solution is hot, and removing alkali insoluble substances and other impurities by adopting a 4-micron sand core funnel to obtain a clear and transparent rubidium carbonate solution.
Step C, disproportionation reaction: and (3) slowly pouring 549.5g of iodine simple substance with the molar ratio Rb: I of 1:1 into the rubidium carbonate solution obtained in the step B under the condition of stirring at normal temperature for carrying out disproportionation reaction, and stirring for 18min to generate a dark brown solution.
Step D, hydrazine hydrate reduction reaction: and C, slowly adding 68.5g of hydrazine hydrate with the mass fraction of 80% into the dark brown solution obtained by the reaction in the step C at normal temperature, controlling the adding rate of the hydrazine hydrate to be 0.4g/s, ending the reaction when the solution is neutral and colorless and no bubbles are generated, finally adding a small amount of hydrazine hydrate to enable the pH of the solution to be 9, and stirring for reacting for 1.5 hours.
Step E, filtering and removing impurities: and D, filtering the solution with the pH of 9 obtained in the step D while the solution is hot at normal temperature, and removing alkaline insoluble substances and other impurities by using a 4-micron sand core funnel to obtain a clear and transparent rubidium iodide solution.
Step F, normal pressure evaporation and concentration: and E, evaporating and concentrating the filtered solution obtained in the step E under normal pressure to 115 ℃ to obtain rubidium iodide slurry.
Step G, cooling and crystallizing: and F, cooling the rubidium iodide slurry obtained in the step F to 45 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal.
Step H, recrystallization and impurity removal: and D, dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1:2, filtering after the rubidium carbonate crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material.
Step I, drying, crushing and packaging: and (3) putting the wet rubidium iodide material obtained in the H into a forced air drying oven, and performing vacuum drying for 3 hours at 170 ℃ to obtain the high-purity anhydrous rubidium iodide. The detection shows that the main content is 99.98 percent, and the water content is 120 ppm.
Example 3:
step A, dissolving rubidium carbonate: at normal temperature, 600g of rubidium carbonate is put into a reaction vessel, 2400g of pure water is slowly added while stirring, and the mixture is stirred for 30min until the rubidium carbonate is completely dissolved.
And B, filtering and removing impurities: and (3) filtering the solution obtained in the step (A) at normal temperature while the solution is hot, and removing alkali insoluble substances and other impurities by using a sand core funnel of 5um to obtain a clear and transparent rubidium carbonate solution.
Step C, disproportionation reaction: and (3) slowly pouring 659.4g of iodine simple substance with the molar ratio Rb: I of 1:1 into the rubidium carbonate solution obtained in the step B under the condition of stirring at normal temperature for carrying out disproportionation reaction, and stirring for 20min to generate a dark brown solution.
Step D, hydrazine hydrate reduction reaction: and C, slowly adding 81.3g of hydrazine hydrate with the mass fraction of 80% into the dark brown solution obtained by the reaction in the step C at normal temperature, controlling the adding rate of the hydrazine hydrate to be 0.5g/s, ending the reaction when the solution is neutral and colorless and no bubbles are generated, finally adding a small amount of hydrazine hydrate to enable the pH of the solution to be 8, and stirring for reacting for 2 hours.
Step E, filtering and removing impurities: and D, filtering the solution with the pH of 8 obtained in the step D while the solution is hot at normal temperature, and removing alkali insoluble substances and other impurities by using a sand core funnel of 5um to obtain a clear and transparent rubidium iodide solution.
Step F, normal pressure evaporation and concentration: and E, evaporating and concentrating the filtered solution obtained in the step E under normal pressure to 120 ℃ to obtain rubidium iodide slurry.
Step G, cooling and crystallizing: and F, cooling the rubidium iodide slurry obtained in the step F to 50 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal.
Step H, recrystallization and impurity removal: and D, dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1:2.5, filtering after the rubidium carbonate crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material.
Step I, drying, crushing and packaging: and (3) putting the wet rubidium iodide material obtained in the H into a forced air drying oven, and performing vacuum drying for 2 hours at 180 ℃ to obtain the high-purity anhydrous rubidium iodide. The detection shows that the main content is 99.97 percent, and the water content is 140 ppm.
The technical indexes of the high-purity anhydrous rubidium iodide product of the above example are shown in the table (1)
TABLE 1 analysis of the quality of the high-purity anhydrous rubidium iodide product
From the above examples and the analysis results of the product components, it can be seen that the method for preparing high-purity anhydrous rubidium iodide of the present invention is simple, easy to operate, low in production cost, and the obtained product has high purity and stable quality.
The above description is only for the purpose of illustrating specific embodiments of the present invention, and should not be construed as limiting the scope of the present invention, and all equivalent changes and modifications made in accordance with the spirit of the present invention should be considered as falling within the scope of the present invention.
Claims (7)
1. A preparation method of high-purity anhydrous rubidium iodide is characterized by comprising the following steps: the method comprises the following steps:
step A: under the condition of normal temperature, 400-600 g of rubidium carbonate is placed into a reaction vessel, pure water with the mass liquid-solid ratio of 2-4: 1 is slowly added while stirring, and the mixture is stirred for 10-30 min until the rubidium carbonate is completely dissolved;
and B: at normal temperature, filtering the solution obtained in the step A while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium carbonate solution;
and C: at normal temperature, slowly pouring an iodine simple substance with a molar ratio of Li to I of 1:1 into the rubidium carbonate solution obtained in the step B under the stirring condition for carrying out disproportionation reaction, and stirring for 15-20 min to generate a dark brown solution;
step D: at normal temperature, slowly adding 80% hydrazine hydrate by mass into the dark brown solution obtained by the reaction in the step C, controlling the addition rate of the hydrazine hydrate to be 0.3-0.5 g/s, ending the reaction when the solution is neutral and the solution is colorless and has no bubbles, and finally adding a small amount of hydrazine hydrate to ensure that the pH value of the solution is within the range of 7-9, and stirring for reaction for 1-2 hours;
step E: at normal temperature, filtering the solution with the pH of 7-9 obtained in the step D while the solution is hot, and removing alkaline insoluble substances and other impurities by using a sand core funnel of 1-5 um to obtain a clear and transparent rubidium iodide solution;
step F: evaporating and concentrating the rubidium iodide solution obtained in the step E under normal pressure, removing a certain amount of water, and concentrating to 105-125 ℃ to obtain rubidium iodide slurry;
step G, cooling the rubidium iodide slurry obtained in the step F to 40-50 ℃, separating out a rubidium iodide crystal material, and then filtering to obtain a rubidium iodide crystal;
step H, dissolving the rubidium iodide crystal obtained in the step G and pure water according to a solid-to-liquid ratio of 1: 1-2.5, filtering after the rubidium iodide crystal is completely dissolved, and repeating the step F and the step G to obtain a rubidium iodide wet material;
and step I, putting the wet rubidium iodide material obtained in the step H into a forced air drying oven, and drying the wet rubidium iodide material in vacuum for 2-4 hours at the temperature of 150-180 ℃ to obtain high-purity anhydrous rubidium iodide.
2. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 1, wherein the method comprises the following steps: and B, preparing the pure water added in the step A into a rubidium carbonate solution with the mass fraction of 20.0% -33.3% by being 2-4 times that of the rubidium carbonate.
3. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 2, wherein the method comprises the following steps: in the step C, the dosage of the iodine simple substance is 1:1 in the molar ratio of Rb to I, and the reaction is completed within 15-20 min.
4. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 3, wherein the method comprises the following steps: said hydrazine hydrate is added in excess in said step D, the solution being weakly alkaline.
5. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 4, wherein the method comprises the following steps: and step B, the aperture of the sand core funnel adopted for filtering and removing impurities in step E is 1-5 um.
6. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 5, wherein the method comprises the following steps: and G, filtering at room temperature by adopting a sand core funnel of 5-15 um.
7. The method for preparing high-purity anhydrous rubidium iodide as claimed in claim 6, wherein the method comprises the following steps: and the drying temperature in the step H is 160-170 ℃.
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