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INVENTION
Patent of the Russian Federation RU2040565
METHOD OF EXTRACTING RUBY FROM SOLUTIONS OF COMPLEX CHEMICAL COMPOSITION
The name of the inventor: Glushankova IS; Kolesova SA; Balandina LV; Volhin V.V.
The name of the patent holder: Perm State Technical University
Address for correspondence:
Date of commencement of the patent: 1991.02.19
Use: the preparation of salts of rare alkali metals. SUMMARY OF THE INVENTION: Rubidium from solutions of a complex chemical composition is sorbed onto a ferrocyanide sorbent, the sorbent is treated with the removal of Rb into the solution in two stages: in the first stage, a chlorine solution in a fluorine-containing organic solvent, which uses fluorinated fluids F-12, F-13, The second is a concentrated aqueous solution of monohydric alcohols, which use an ethyl alcohol with a concentration of 85 96% v / v. Or isopropyl with a concentration of 80 88% vol. Rubidium chloride is obtained by evaporating the solution, distilling off the alcohols and reusing them.
DESCRIPTION OF THE INVENTION
The invention relates to methods for the preparation of salts of rare alkali metals and can be used in technology for the preparation of rubidium salts.
A sorption method is known for extracting rubidium ions from solutions of a complex chemical composition with a high content of alkali and alkaline earth metal salts, using ferrocyanides (hexacyanoferrates) of transition metals Ni (II), Cu (II) as sorbents, followed by desorption of rubidium ions and processing of eluates by known methods By evaporation or precipitation in the form of a sparingly soluble compound) [1,2]
It is known that ferrocyanides of transition metals selectively extract rubidium ions from solutions of different composition, with high separation coefficients of Rb + and K + , Rb + and Na + (K p 10 3 ) ions [2,3]
However, the widespread use of sorption technology for the preparation of rubidium salts is constrained by the lack of a sufficiently effective method for desorption of Rb + ions from the ferrocyanide composition, which simultaneously creates difficulties for obtaining rubidium salts of reactive qualification.
There are known ion-exchange methods for the desorption of Rb + ions and other alkali metals from the composition of ferrocyanide sorbents with the help of ammonium chlorides or nitrates [3] However, these methods are ineffective. There are also known methods of desorption of ions of alkali metals and thallium (I) from the composition of ferrocyanides with the use of oxidizing agents. As the oxidizer, highly concentrated solutions of nitric or sulfuric acids are used [4]
The closest to the proposed technical solution (prototype) is a method for isolating rubidium, which includes the sorption of rubidium on the ferrocyanide sorbent and subsequent treatment of the sorbent with the extraction of rubidium into the solution, to obtain a solution of rubidium chloride [3]
However, as a result of desorption, significant volumes of eluates with a low concentration of rubidium are formed, which leads to high energy costs when processing solutions to obtain rubidium chloride. In addition, to obtain a sufficiently pure salt, preliminary separation of Rb + and Na + ions is required , which complicates the technology.
The purpose of the invention is to increase the degree of extraction of rubidium into the product and to reduce energy consumption.
The goal is achieved by desorption of Rb ions from the ferrocyanide composition by treating the latter with a solution of chlorine in an organic solvent. The liberated rubidium chloride is transferred to the solution by concentrated aqueous solutions of low-boiling monohydric alcohols, followed by distillation by evaporation and obtaining highly concentrated solutions of the rubidium salt. The distilled alcohol is reused for the desorption of rubidium in the next cycle of sorbent operation.
Fluorine fluids, for example F-12, F-13, are chosen as the chlorine solvent, which meet the following requirements: low volatility, incombustibility, high chemical inertness (oxidant resistance), low solubility in water and alcohols, nontoxicity. The saturation with chlorine of the organofluorine liquids was carried out in a known manner, passing the gaseous chlorine through a solvent. At room temperature, the equilibrium concentration of chlorine in F-12, F-13 is 0.5-0.7 M. The high concentration of chlorine in the solution makes it possible to significantly reduce the amount of eluent necessary for the desorption of rubidium ions from the ferrocyanide composition. The extraction of rubidium chloride isolated from the sorbent is carried out with water or alcohol solutions. Roubidium chloride dissolves in monohydric alcohols (methyl, ethyl, propyl, isopropyl, etc.) and their aqueous solutions.
In order to reduce the energy consumption for evaporation of the eluates, it is proposed to desorb RbCl chloride with solutions of ethyl or isopropyl alcohols, which are chosen taking into account low boiling point and low toxicity. The heat costs for obtaining 1 kg of the rubidium salt by evaporating the eluates were calculated by the formula
Example 1 . 5 g of ferrocyanide sorbent, the gross formula of which K 0.92 Cu 1.54 [Fe (CN) 6 ] 4.9 SiO 2 , was loaded into an ion exchange column 0.7 cm in diameter and a sorbent layer height of 20 cm, and sorption of Rb from A model solution containing rubidium and potassium chlorides with a ratio of Rb + : K + 1: 150 and a concentration of Rb of 0.2-0.25 g / l (2.34 .10 -3 -2.9 .10 -3 ) at a rate of Passing a solution of 2-3 columns / h. The total ion-exchange capacity of the sorbent for the ion Rb was 0.82-0.88 mmol / g sorbent. At the same time, the separation coefficients of Rb + K + ions reached 5 . 10 3 5.5 . 10 3 .
To obtain the rubidium salt of reactive qualification, selective desorption of K + and Rb + was carried out .
The desorption of potassium ions from the ferrocyanide was carried out with a 1 M hydrochloric acid solution. With the passage of 8-10 column volumes (KO) of the eluent, almost complete desorption of K + is achieved, while the recovery of Rb ions is less than 1%
The concentration of rubidium and potassium ions was measured by the atomic absorption method.
To extract rubidium from the sorbent composition, the latter was treated with a 0.7 M chlorine solution in fluorinated F-13 liquid by passing it through an ion-exchange column at a rate of 3-4 KO / h. The complete oxidation of the sorbent was controlled by the consumption of chlorine. The chlorine concentration in the organic solvent was measured by the titrimetric method. For the complete oxidation of ferrocyanide, 2 KO of chlorine solution was required. Then water was passed through the sorbent to separate the formed rubidium chloride at a rate of 4-5 KO / h. Samples of eluate for analysis were selected by fractions of 20 ml. For complete desorption of Rb ions, 8 KOs were required. The first eluate fraction with the maximum concentration of the main component was processed into a finished product, and the following fractions were collected and reused for desorption of Rb ions in the following cycles.
After the desorption process, the sorbent was washed with 2-3 KO water, regenerated in a known manner and used in the next rubidium sorption cycle [4]
The concentration of rubidium chloride in the first fraction of the eluate and the heat costs for its evaporation are shown in the table.
Example 2 . Sorption of Rb + ions and desorption of K + ions was carried out according to Example 1. To transfer RbCl to the eluate, ethyl alcohol with a concentration of 96 vol. For complete desorption of RbCl, 12 KO of alcohol were required. The concentration of RbCl in the first fraction of the eluate and the approximate heat costs for obtaining 1 kg of the rubidium salt are shown in the table.
Example 3 . Sorption of Rb + ions and desorption of K + ions was carried out according to Example 1. The sorbent was then treated with a 0.4 M chlorine solution in fluorinated liquid F-13. The eluent consumption, which is necessary for the complete oxidation of the sorbent, was 3-4 KOs. The sorbent was then treated with a solution of ethanol at a concentration of 84 vol. For complete isolation of RbCl, 8 KO of eluent was passed. The results of desorption are presented in the table.
Example 4 . Sorption of Rb + ions and desorption of K + ions was carried out according to example 1. The sorbent was then treated with a 0.5 M chlorine solution in F-13. The eluent solution was 2-3 KO. Then, 70 vol.% Was passed through the column to extract RbCl through the column. Solution of ethyl alcohol, in an amount of 6 KO. The results for desorption of RbCl are presented in the table.
Example 5 . Sorption of Rb + ions, desorption of K + ions, treatment of the sorbent with chlorine solution was carried out according to Example 1. RbCl desorption was carried out with a 100% solution of isopropyl alcohol, 12 KO of alcohol was required to completely remove RbCl. The results of the experiment are presented in the table.
Example 6 . Sorption of Rb + ions, desorption of K + ions, treatment of the sorbent with a chlorine solution was carried out according to Example 1. For desorption of RbCl through a sorbent, 10 KO of isopropyl alcohol with a 95% concentration were passed. The results of the experiment are shown in the table.
Example 7 . Sorption of Rb + ions and desorption of K + ions was carried out according to Example 1. The sorbent was then treated with a 0.5 M chlorine solution in fluorinated F-12 liquid. To completely oxidize the sorbent, it took 3 KO of the eluate. To remove RbCl through the column, 8 KO of 88 vol. Solution of isopropyl alcohol. The results of the experiment are presented in the table.
Example 8 . Sorption of Rb + ions, desorption of K + ions, and sorbent treatment with chlorine were carried out according to example 1. Then, 66 KOs of 80 vol.% Were passed through the column to recover RbCl. Solution of isopropyl alcohol.
The results of the experiment are presented in the table.
Example 9 . The sorption of rubidium ions, the desorption of K + ions, and the treatment of the sorbent with chlorine were carried out according to example 1. Then, to remove RbCl through the column, 4 KO 75 vol. Solution of isopropyl alcohol. The results of the experiment are presented in the table.
From the data given in the table, it can be seen that the process of desorption of rubidium ions from the ferrocyanide sorbent composition and the preparation of the rubidium salt by evaporating the eluates is most expediently carried out by treating ferrocyanide with a 0.5-0.7 M chlorine solution in fluorinated liquid F-12 or F-13, and then The chloride of rubidium released from the sorbent phase is extracted with a 96-85% solution of ethyl or 88-80 vol. Solution of isopropyl alcohols.
The use of water to extract rubidium chloride from the sorbent composition is inadvisable because of the high energy costs in obtaining salt by evaporating aqueous solutions.
The use of less concentrated solutions of alcohols for desorption of rubidium ions reduces the concentration of this ion in solutions obtained after distillation of alcohol and increases energy consumption during their processing. The use of more concentrated solutions of alcohols is ineffective due to the low solubility of rubidium salts in them.
The proposed method for extracting rubidium from complex solutions allows, in comparison with the prototype, to increase the concentration of rubidium in the eluates 1.5-2 times and to reduce energy consumption for obtaining a rubidium salt by a factor of 3-6.
CLAIM
1. A method for extracting rubidium from solutions of complex chemical composition, comprising sorbing rubidium on a ferrocyanide sorbent and subsequently treating the sorbent with extracting rubidium into a solution to obtain rubidium chloride, characterized in that, in order to increase the degree of extraction of rubidium into the product and reduce energy consumption, treatment of the ferrocyanide Sorbent is conducted in two stages, in the first stage with a solution of chlorine in a fluorine-containing organic solvent, in a second concentrated aqueous solution of monohydric alcohols, followed by distillation by evaporation and reuse.
2. A process according to claim 1, characterized in that fluorinated fluids F-12, F-13 are used as the fluorine-containing organic solvent.
3. A process according to claim 1, characterized in that monohydric alcohols use ethyl at a concentration of 85-96 vol. Or isopropyl with a concentration of 80-88 vol.
print version
Date of publication 15.03.2007гг
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