Method of granulating lithium salts
(57) Abstract:The invention relates to methods of granulation lithium salts. The invention consists in that in the chamber and injected lithium salt, create mode "fluidized bed" by supplying heated fluid and creates a vacuum in the range of 5-40 mm water.article Through a nozzle by means of compressed air supplied to the solution of lithium salts and granularization. Increasing the height of the fluidized-bed forming granules of lithium salts come in a host acceptance, and pulverized fraction by means of the exhaust fan is directed into the absorber, and then for further processing. The method allows to obtain granules of lithium salts, particularly chloride, lithium bromide, resistant to destruction, and to increase the yield. 9 C.p. f-crystals, 2 Il. The invention relates to the field of chemical industry, in particular to methods of granulation lithium salts, intended for the production of lithium salts.Lithium salts are usually obtained from lithium carbonate, or by reacting with acids. Almost all alkali metal salts dissolve easily in water. Only lithium forms several relatively insoluble salts. Ions of the alkali metal is in nformation contain water molecules. Because of this, and packaging of lithium salts has always received special attention.There is a method of granulating salts of alkali metals, according to which a mixture of sulfate and potassium chloride is melted and granularit, resulting in contact with the rotating cooling surface (see WO 96/29287, A1, Dead Sea Works LTD. , 26.09.96, C 01 D 3/22), the lack of which is the fact that when granulating lithium salts, the final product is unstable, easily decomposed and inconvenient for storage and further use.The closest in technical essence and the achieved result is a method of granulating lithium salts, including the introduction of salts into the camera, the processing of reagent water in the turbulent flow regime, the formation of granules and release of granules from the camera (see US, 4320105, A Lithium Corporation of America, 16.03.82, C 01 D 15/00) prototype. The disadvantage of this method is the low quality pellets lithium salts and low yield of the final product.An object of the invention is to create a method of producing granules of lithium salts, which would allow it to increase their resistance to damage, ultimately leading to improved conditions and increased yield about is the introduction of salts into the chamber, the processing of reagent water in the turbulent flow regime, the formation of granules and release of granules from the camera, according to the invention, the processing of the salts is carried out in the presence of granulomatous, as water reagent is used, the lithium salt solution, and the processing of the salts is carried out in the mode of "fluidized bed" with compressed air, with dust-like fraction of lithium salts are removed from the chamber for further processing.The technical result in the maximum level is achieved when the following conditions are met:
as granulomatous use carbamide hydrogen peroxide or other granularization, which picked empirically for a specific lithium salts;
as the lithium salt solution use solutions of lithium chloride, bromide or other salts;
- processing of salts is carried out at a pressure in the chamber 5-40 mm water column;
as the coolant serves the air heated to a temperature of 380-420oC;
a solution of a lithium salt served in dispergirovannom condition;
the lithium salt solution is fed through a nozzle in a stream of compressed air;
- an aqueous solution of lithium salts and granularization serves at the same time;
- water plants is the Ktsia lithium salts are removed from the chamber through the openings in the absorber for further use as a source of raw materials.In Fig. 1 shows a device for granulating lithium salts. The installation includes a camera 1 "fluidized bed", Luke 2 download lithium salts, node 3 acceptance of granules, the pipe 4 for feeding the heat carrier and the absorber 5 to derive pulverulent fraction of lithium salts. The fan 6 is used to create vacuum in the chamber, Tara 7 - for packing of lithium salts.In Fig.2 presents a photograph of the finished product granules lithium salts.The essence of the proposed method is illustrated by examples of its implementation.Example 1.In the camera 1 "fluidized bed" in line 4 serves the air heated to a temperature of 400oC, by means of the exhaust fan 6 generate a vacuum of 15 mm of water column. Through Luke 2 download lithium chloride and lithium hypochlorite (LiOCl) for activation of the reaction (in small quantities). In the lower part of the chamber through a nozzle (not shown) serves an aqueous solution of lithium chloride in a stream of compressed air. Before serving in a solution of lithium chloride added urea ((NH2)2CO). Under these conditions, the camera fluidized-bed 1 place the following reactions:
< / BR>Molecules hydrazine (N2NK4) are the active centers granulometry lithium chloride in node 3 of acceptance and further transported in the packaging container 7.In fluidised bed combustion chamber 1 part pellets used up, forming a dust-like fraction. By means of the exhaust fan 6 pulverulent fraction catch in the absorber 5, from which connections are sent for recycling.Example 2.Under the conditions described in example 1, the camera 1 is injected lithium bromide. Through a nozzle serves an aqueous solution of lithium bromide in the compressed air. Before serving in a solution of lithium bromide add the hydrogen peroxide In the chamber 1 "fluidized bed" hydrogen peroxide is destroyed by the following reactions:
Atomic oxygen is the active center granulometry of lithium bromide.The size of the granules depends on the dimensional parameters of the working parts of the camera 1 "boiling layer" and can be changed by varying the feed mode aqueous solution of lithium salts and granularities.The use of the proposed method increases the quality of pellets lithium salts by increasing their resistance to destruction and, consequently, to improve conditions and increase yield. 1. Method of granulating lithium salts, including an introduction to the camera, processing the the action scene, that the processing of the salts is carried out in the presence of granulomatous, as water reagent is used, the lithium salt solution, and the processing of the salts is carried out in the mode of "fluidized bed" with the supply of coolant and compressed air, with dust-like fraction of lithium salts is removed from the camera.2. The method according to p. 1, characterized in that as granulomatous use carbamide hydrogen peroxide.3. The method according to p. 1, characterized in that as the aqueous reagent use solutions of salts of chloride, bromide lithium.4. The method according to p. 1, characterized in that the processing of the salts is carried out at a pressure in the chamber 5-40 mm water. Art.5. The method according to p. 1, characterized in that the coolant serves the air heated to a temperature of 380-420oC.6. The method according to p. 1, wherein the lithium salt solution served in dispergirovannom condition.7. The method according to p. 1, wherein the lithium salt solution is fed through a nozzle in a jet of compressed air.8. The method according to p. 1, characterized in that an aqueous solution of lithium salts and granularization serves at the same time.9. The method according to p. 1, characterized in that an aqueous solution of lithium salts, granulate pulverized fraction of lithium salts are removed from the chamber through the openings in the absorber for further processing.
FIELD: chemical technology and non-ferrous metallurgy; production of lithium-containing fluorides for electrolytic production of aluminum.
SUBSTANCE: proposed method includes selective sorption of lithium from natural salting liquor followed by desorption of it with water, thus obtaining eluate, solution LiCl containing also CaCl2 and MgCl2 at ratios dictated by composition of salting liquor. Then eluate is concentrated, treated with water and Li, Mg and Ca carbonates settle, after which they are subjected to treatment with hydrofluoric acid for obtaining mixture of LiF, MgF2 and CaF2. Proposed method may be also realized by settling Mg and Ca carbonates from starting liquor by soda solution for obtaining mixture of MgCO3 and CaCO3 at low content of Li2CO3 and lithium carbonate is added to this mixture in the amount of 30-50% of mass of total content of components; then mixture is stirred and treated with hydrofluoric acid for forming LiF, MgF2 and CaF2 fluorides at content of LiF from 30 to 50%. Used as fluorine-containing reagent is hydrofluoric acid, gaseous fluorine and/or gaseous hydrogen fluoride. Use of natural salting liquor makes it possible to obtain fluorides at minimum content of K, Si and Cl admixtures, not exceeding 0.2% of masses.
EFFECT: enhanced efficiency.
4 cl, 2 dwg, 10 ex
FIELD: production of lithium chloride.
SUBSTANCE: proposed method includes interaction of lithium carbonate in form of aqueous suspension with chlorine in double-stage absorbers in presence of iron-nickel catalyst, cleaning from admixtures, evaporation and drying. Lithium carbonate aqueous suspension used for realization of this method has mass ratio to water of from 1:5 to 1:6.5; process is continued to content of lithium chloride in liquid phase between 180-220 g/l at transformation of solution into acid medium to pH lesser than 7 and periodic change of delivery of chlorine-air mixture from first absorption chain to second and vice versa. Cleaning from admixtures of potassium, sodium, calcium and barium is performed through contact of two liquid phases- lithium amalgam and aqueous solution of lithium chloride which interact in contact system in counter-flow; contact system consists of several columns with vinyl plastic Raschig rings packing. Lithium contained in amalgam is shifted to aqueous solution upon escaping from contact system by passing the amalgam in contact with water through amalgam decomposer, after which lithium hydroxide solution is introduced into contact system in counter-flow relative to amalgam where it is mixed with flow of aqueous solution of lithium chloride introduced into contact system for cleaning. Aqueous solution of mixture of lithium chloride and lithium hydroxide escaping from contact system is directed to third and fourth finish chains of absorption where repeated chlorination is carried out.
EFFECT: reduction of labor input; reduction of power requirements; enhanced cleaning.
1 dwg, 3 tbl
FIELD: chemical industry; other industries; methods of production of the electrolyte component on the basis of lithium hexafluorophosphate.
SUBSTANCE: the invention is pertaining to the method of production of the electrolyte component for the lithium sources of the electric current. The method of production of the electrolyte component on the basis of lithium hexafluorophosphate provides for the reaction of pyridinium hexafluorophosphate with lithium hydroxide in the dissolvent with the topping of the volatile fractions in the vacuum. In the capacity of the dissolvent use propilencarbonate. After termination of the reaction without the individual extraction of the lithium hexafluorophosphate conduct the azeotropic drying of the received solution. Then exercise the topping of the volatile products of the reaction with a part of propilencarbonate and formation of the lithium hexafluorophosphate in the propilencarbonate with its concentration corresponding to the saturated solution at the room temperature. The technical result of the invention is production of the component of the electrolyte in the form of the solution of the salt - LiPF6 in the suitable dissolvent.
EFFECT: the invention ensures production of the component of the electrolyte in the form of the solution of the salt - LiPF6 in the suitable dissolvent.
5 cl, 4 ex
SUBSTANCE: method of lithium chloride purification from admixtures involves obtaining processing medium of lithium chloride with lithium oxychloride residues by dissolution of processing lithium hydroxide in water or by preparation of processing lithium carbonate slurry, followed by chlorination of lithium hydroxide solution or lithium carbonate slurry by waste chlorine air mix of electrolytic cells in the presence of a catalyst used for lithium oxychloride reduction. pH of the obtained lithium chloride solution is corrected before continuous sorption purification with lithium hydroxide solution or lithium carbonate till hydroxyl ion (OH-) content is within 0.0002-0.005 mol/dm3. Lithium chloride solution undergoes sorption purification with cation exchange resin based on cross-linked macroporous polystyrol featuring subacid iminodiacetate groups inserted into the polymer matrix of subacid iminodiacetate groups with linear throughput rate of 3-20 m/h. The method improves purity degree of the processing lithium chloride solution and prolongs performance lifetime of cation exchange resin.
EFFECT: purified lithium chloride solution allows obtaining high-quality metal lithium.
2 ex, 1 tbl, 3 dwg
SUBSTANCE: method of obtaining high-purity lithium fluoride from processing lithium compounds, such as lithium carbonate or hydroxide, involves transition of the compounds to lithium hydrocarbonate solution by processing of their water solutions by carbon dioxide, sorption purification of the lithium hydrocarbonate solution by cation exchange resin, obtaining of purified lithium carbonate, its washing, preparation of water slurry of purified lithium carbonate, repeated bicarbonisation of water lithium carbonate slurry by carbon dioxide, obtaining of lithium hydrocarbonate solution, followed by fluorination, washing and drying of obtained lithium fluoride. Fluorination is implemented by slow addition and continuous stirring of lithium hydrocarbonate solution in a reactor filled with fluorine hydride with 10-30% stoichiometry excess. Lithium fluoride is washed by distilled water without CO2 or by 1% solution of fluorine hydride. Lithium fluoride is dried in two stages in vacuum furnace, first stage drying temperature is under 100°C, and second stage drying temperature is under 150°C.
EFFECT: obtaining lithium fluoride with high content of the main substance.
3 ex, 2 tbl, 3 dwg
SUBSTANCE: invention relates to production of fluoride salts, particularly to a method of producing lithium hexafluorophosphate. The method involves mixing a lithium-containing compound which does not contain fluorine, a phosphorus-containing compound and a fluorinating agent. The phosphorus-containing compound used is phosphorus oxide which is taken in stoichiometric ratio to the lithium-containing compound. The fluorinating agent used is ammonium fluoride or hydrofluoride, which is taken in excess of up to 20% of the stoichiometric ratio. The obtained mixture is heated to 200°C until complete separation of gaseous reaction products.
EFFECT: reduced number of steps for obtaining lithium hexafluorophosphate, use of readily available, solid reagents which do not need further processing.
SUBSTANCE: invention relates to chemistry. Lithium-bearing natural brines undergo enrichment on sorption-desorption module with obtaining primary lithium concentrate. To obtain secondary lithium concentrate primary lithium concentrate is concentrated by natural way, after which solution undergoes reagent purification and purification on polyampholyte; or lithium concentrate first undergoes ion-exchange purification, purified lithium chloride solution is subjected to reverse osmosis concentration, intermediate lithium concentrate undergoes evaporation and reagent purification; or concentrate undergoes purification from magnesium and calcium admixtures in contact with lithium carbonate, purified lithium chloride solution is concentrated first in reverse osmosis way with obtaining intermediate lithium concentrate, after that, intermediate lithium concentrate is evaporated to desalt NaCl and subjected to reagent purification; lithium concentrate undergoes ion-exchange purification from magnesium and calcium admixtures, purified solution of lithium and sodium chlorides undergoes reverse osmosis concentration, intermediate concentrate undergoes thermal desalting of NaCl; obtained lithium chloride solution is diluted and subjected to reagent purification. Obtained secondary lithium concentrate is used to obtain lithium carbonate or chloride, or fluoride, or lithium bromide, or lithium hydroxide monohydrate.
EFFECT: invention makes it possible to process lithium-bearing concentrate in complex way.
5 cl, 4 dwg, 2 tbl, 17 ex
SUBSTANCE: method for lithium chloride regeneration in chemical industry comprises plasticization and precipitation bath solution neutralisation with an aqueous solution of lithium hydroxide. Multicomponent starting mixtures contain 0 to 60% of dimethylacetamide (DMAA), 0 to 70% isobutyl alcohol (IBA), lithium chloride, hydrogen chloride, water and impurities - balance to 100%. These mixtures were separated to lithium chloride containing ones and not containing ones. The mixtures which do not contain lithium chloride are separated to mixtures containing DMAA and mixtures not containing DMAA. The liquid stream consisting of IBA and water is removed from the system. At that, the plasticization bath solution is rectified in two columns and the distillation residue mixture of the second column and the precipitation bath is evaporated by vacuum. Vacuum rectification of vacuum evaporator distillation residue, vacuum rectification of vacuum evaporator and the third column stripping product is performed to obtain dimethylacetamide (DMAA). The concentrated lithium chloride solution is crystallized in dimethylacetamide. The flow of concentrated lithium chloride is sequentially fed to vacuum rectification, crystallization and centrifugation. Lithium chloride complex salt - dimethylacetamide - is separated from the stock solution. Purified lithium chloride is obtained from the stock solution by repeated dilution with water and vacuum evaporation.
EFFECT: invention allows to obtain lithium chloride with a purity up to 95 percent and a high yield.
FIELD: chemical industry, agriculture, in particular hardness removal agent and saltlick for cattle.
SUBSTANCE: salt with pH 4-10 is pressed under 5000-2500 N/cm2. Salt contains NaCl, less than 0.1 wt.% of water, and iron-ammonium complex of polyhydroxycarboxylic acid in amount sufficient to obtain non-caking salt. As iron-ammonium complex of polyhydroxycarboxylic acid iron-ammonium citrate with molar ratio of iron to citrate-ion from 0.5 to 2 and molar ratio of ammonium to citrate-ion from 0.5 to 2 may be used. Finished product contains 0.1-20 mg/kg of iron and has form of briquettes, balls, bars, crushed plates, tablets, etc. Invention makes it possible to provide good formability under high pressure and conserve pressed product shape in moist medium for a long time.
EFFECT: products from salt non-caking at storage and conveyance.
11 cl, 6 tbl, 2 dwg, 7 ex
FIELD: materials for miscellaneous applications.
SUBSTANCE: grain mixture comprise, in mass %, 15-45% of compressed first salt of alkaline or alkaline-earth metal and 85-55% of the second salt of alkaline or alkaline-earth metal. The first salt is a waterless hygroscopic salt.
EFFECT: reduced cost.
14 cl, 4 dwg
SUBSTANCE: invention refers to the method for preparation of moisture resistant potassium chloride with enhanced rheological properties. The method includes compression of the concentrated potassium chloride obtained by the halurgic or flotation concentration of the sylvinite ore with the additive of the mineral substance. The aforesaid mineral substance is structure-forming salt selected from the potassium or sodium carbonate, sulphate, dihydroorthophosphate, orthophosphate or metasilicate, it is fed to the wet concentrate in the stage of structural agglomeration before drying. The latter stage is carried out at moisture level 3.0 - 5.0% in turbo-bladed mixer-granulator by the way of plastic deformation of the wet concentrate mixed with dry hot potassium chloride. The structure-forming salt is fed in amounts of 0.5 - 5.0 kg/t of the ready product (dry or in the form of water solution). The dry hot potassium chloride is fed to the stage of plastic deformation in amounts of 10 - 20% in relation to the weight of the dry agglomerated potassium chloride.
EFFECT: method is versatile and allows to obtain the fine and compression granulated potassium chloride which is able without treatment with anti-clodding agent to retain its grain size composition and flowability at storage and handling in wet climate.
4 cl, 4 tbl, 1 ex
SUBSTANCE: invention can be used in chemical industry. The method of producing granular potassium chloride involves structural agglomeration of filtered potassium chloride in a turbo blade mixer-granulator, drying and pressing the agglomerated product, grinding the pressed product and sizing the ground product. Structural agglomeration of the potassium chloride is carried out together with fine sizes of the granulation stream obtained after sizing the ground pressed product with the load on the turbo blade mixer-granulator not less than 400 t/m2 of its cross section. The agglomeration process is not shorter than 15 seconds.
EFFECT: invention enables to obtain granular potassium chloride with improved rheological properties such as static strength and wearing capacity of granules, not contaminated with structure-forming additives.
2 tbl, 2 ex
SUBSTANCE: invention can be used in producing halurgic potassium chloride from sylvinite ore using a dissolution-crystallisation method. The method of producing potassium chloride involves structural agglomeration of a mixture of a wet crystallisate and dry hot potassium chloride in a mixer-granulator and then drying the mixture. For structural agglomeration of the mixture, dry hot potassium chloride is fed in amount of 25-100% of the weight of wet crystallisate. The mixture is dried at temperature 105-135°C to obtain the end product.
EFFECT: invention reduces caking capacity of potassium chloride, avoids use of structure-forming salts, reduces consumption of reagents used to prevent potassium chloride from caking, and obtain a product which does not contain extraneous impurities.
2 cl, 2 tbl, 2 ex