Method of production of platinum metals nanoparticles

FIELD: technological processes.

SUBSTANCE: method includes preparation of direct or reverse micelles with further reduction of metal precursors in them. Prior to preparation of micelles they are concentrated from water solutions by means of ion flotation or flotation extraction with application of surface agents and hydrocarbons. As water solutions artificial mixtures of dissolved water solutions are used, sewage waters, solutions of ores or their wastes that are poor in platinum metals, solutions of anode slimes of metals electrolytic cleaning.

EFFECT: preparation of platinum metals nanoparticles from wastes of mining industry; ores poor in platinum metals and sewage waters.

2 cl

 

The invention relates to a process for producing nanoparticles hybrids (alloys) of platinum metals with other metals. Nanoparticles can be used as catalysts, magnetic and other materials.

Known to produce metals and hybrids of metals in reverse micelles (M.P. Pileni // Langmuir, V.13, R-3276). According to the method of preparing a reverse micelle (microemulsions) of aqueous solutions of salts, acids, e.g., H2PtCl6in isooctane in the presence of emulsifier sodium bis(ethylhexyl)sulfosuccinate (AOT). Separately prepare the microemulsion of the reducing agent aqueous solution of hydrazine hydrate is added. Two microemulsions are mixed. In order to prevent oxidation of the reaction mixture, is passed through a mixture of microemulsions nitrogen. In the reaction are formed nanoparticles of platinum.

As precursors in a known method is used pure salts, acids, hydroxides. The disadvantage of this method is the impossibility of obtaining nanoparticles of metals, hybrids metals from waste, poor platinum metals ores, waste waters.

An object of the invention is to obtain nanoparticles of platinum metals from mining wastes, poor platinum metals ores, waste waters.

The technical result is achieved by the fact that, according to the method for producing platinum nanoparticles the x metals including preparation of micelles and subsequent reduction in them precursors of the metals recovery using direct and inverse micelles, and before preparing micelles their concentrate from aqueous solutions by ion flotation or protectable with the use of surface-active substances (surfactants) and hydrocarbons, and after use the resulting solution of the precursor with a surfactant in the hydrocarbon to prepare micelles.

As aqueous solutions using artificial mixtures of dilute aqueous solutions, waste water, poor solutions on platinum metals ores or waste solutions anode slimes electrolytic cleaning of metals.

The invention is illustrated by examples.

Example 1. Decompose the ore composition: carbonaceous shale with striated silicification), containing about 20 g/t platinum, 15 g/t of palladium, 100 g/t of zinc, 500 g/t of copper. A sample of fragmented ore in the amount of 100 g is poured into a Teflon beaker with a mixture of 500 ml of hydrofluoric acid and 50 ml of nitric acid, is stirred, the solution is evaporated at a temperature of 160-200°to wet salts, the remainder of the double-pour 500 ml of Aqua Regia and both times evaporated to moist salts at the same temperature. Then the residue is dissolved in 10 ml of 0.1 M hydrochloric acid. Undecomposed ore is filtered off and discarded. In each of 10 ml of the solution is kept in the form of ions about 20 mg of platinum, 15 mg of palladium, 1 g of copper and 0.5 g of zinc. Ten 10 ml of hydrochloric acid solution of salts of platinum, palladium, copper, zinc merge together and poured into a column for protectable.

Column for photoextract.com is a glass cylinder with a diameter of 30 mm and a height of 500 mm from the bottom of miplasta. Through Siplast as the dispenser is supplied by the air compressor. The air supply is regulated by the valve. For protectable column add alcohol solution reservoir - surface-active substances (surfactants), which form the precursors of the metals lahoratories in water molecules. These molecules adsorbed on the surface of the bubbles and transferred them to the surface of the aqueous solution is isooctane. Hydrocarbon (hexane, heptane, octane, isooctane, benzene, toluene, butylbenzoyl) is poured on top of the aqueous solution. Platinum in acidic solution of hydrochloric acid is in the form of the complex ion [Pt(Cl)6]2-and so can flotirovanija s-dodecylamine chloride [C12H23SC(NH2)2]+Cl (DTCH) or a primary, secondary, tertiary alkylamines followed, forming a salt by ion-exchange mechanism

[C12H25SC(NH2)2]2+[Pt(Cl)6].

This salt is soluble in the hydrocarbon. She gradually concentrated to the desired concentration required for the synthesis of nanoparticles. About the simultaneous DTH platinum palladium. Salts of copper and zinc in aqueous solution are in the form of cations Cu2+, Zn2+. So after flotation of platinum and palladium them platinuum anionic surfactant (alkyl sulphates, alkalicarbonate, tributylphosphate, organophosphorus compounds). For this purpose is the emulsifier AOT. After creating the desired concentration of precursor metals in hydrocarbon (˜0.1 g of platinum, ˜0.15 g of palladium ˜10 g copper, ˜5 g of zinc) hydrocarbons with metal ions and ions of the surfactant is separated from the rest of the solution in a separating funnel and transferred to the reactor for the synthesis of hybrids of platinum with other metals. Most metals, such as cobalt, Nickel, iron, copper, zinc, recovered from aqueous solutions of their salts without the platinum metals. Platinum metals, recovering and crystallizing the first, give the possibility to obtain nanoparticles with other metals. Moreover, the content of platinum metals in hybrids can be small (0.5 to 5%).

The reactor for the synthesis of nanoparticles is a glass stirrer 5000 rpm for preparing reverse micelles. Analyze the content of ions (precursor), ATC, AOT in hydrocarbon solution. AOT is responsible for creating a certain size of microemulsions (micelles). At a molar ratio [H2O]/[AOT] you can judge the size of the pools (water drops) micelli on them to determine the approximate size of the nanoparticles. ATC, which in solution an order of magnitude smaller than AOT, may affect the size of the nanoparticles and their other options. In the solution of precursors in the hydrocarbon add water in the ratio needed to obtain the required size of the nanoparticles. Mix to form a microemulsion in water pools which were precursors in the form of [Pt(Cl)6]2, Cu2+, Zn2+.

Separately prepare a microemulsion based only AOT, isooctane and water, in water pools is hydrazinehydrate. Hydrazinehydrate add 1.5 excess relative to the number of ions. Mixing two microemulsions and let this mixture of nitrogen, which performs the function of an inert atmosphere and at the same time contributes to the stirring reaction mixture. The reaction rate of recovery due to the speed of intermolecular exchange of precursors and hydrazine hydrate is added in the collision of microemulsions, flexible surface film of the microemulsion and other factors. After 0.5-1 hour of stirring in water pools formed nanoparticles hybrids. This mixture of metals cannot be called alloy, as the mixture is obtained by crystallization, and not melting. If micro-emulsions themselves are not destroyed, for their destruction add dimethylformamide or any other solvent: pyridine, dimethylamine, etc. Microemulsions are stratified and on the interfacial behavior of the displacement water the hydrocarbon layer appears a new solvent-nanoparticle hybrids. The nanoparticles are separated by filtration or centrifugation. The dried nanoparticles and determine the composition of atomic absorption spectrometry: 0.18 g of platinum, 0.11 g of palladium, 8.5 g of copper and 4.7 g of zinc. In percent: 1,7% platinum, 0.8% of palladium, 63,0% copper, 34.8% of zinc.

The average size of the nanoparticles is determined on the ultracentrifuge, pre dispersive them in water, according to the formula:

where η - viscosity solvent, PA·C; x0- the initial distance from the axis of rotation of the centrifuge to the center of the tube, m; x is the distance from the axis of rotation of the centrifuge to the center of the tube after settling for a time τ; n is the number of revolutions of the centrifuge, 1/; τ the time of rotation of the centrifuge; ρ is the density of the nanoparticles, kg/m3; ρ0- the density of water, kg/m3; r is the radius of the nanoparticles, nm. Get the diameter of the nanoparticles is 18±2 nm.

Example 2. Take sulphate solution baths anodic dissolution of alloys JSC "Norilsk Nickel". It contains 75 g/l of sulfate ions, 15 g/l chloride ions, 0.24 rhodium, 0.40 ruthenium and 18.8 mg/l iridium. 1 l of a solution is placed in the column for holding of the ion flotation. Add the equivalent of the precursor mixture in 5 ml of ethyl alcohol of decylamine with s-dutilisation chloride in a ratio of 15:1. Platinum metals are in rest the re in the form of ions [e(Cl) 6]2-. The top in the column add octane. After 30 min. transmission of air analyze the content of the precursors of platinum metals in octane: 0,12 mg/l of rhodium, 0.16 mg/l of ruthenium, 5.6 mg/l iridium. Evaporated octane. Of the remaining mixture of salts is prepared an aqueous solution of approximately 5·10-4M eridia. The mixture of salts can be obtained without octane, collecting the foam. There also add with NISO4and cetyltrimethylammonium chloride, to the solution was Ni2+1,4·10-2M, and by cetyltrimethylammonium chloride of 0.3·10-3M Through micellar water solution for 20 minutes to let the nitrogen to remove dissolved oxygen and mixing. After stirring 30 ml of hydrazine hydrate is added and 200 ml of 9 M solution of potassium hydroxide. Must be an excess of potassium hydroxide, which can be verified by analysis. The solution after 15 min of additional stirring, and the reaction was 0.3 M in potassium hydroxide. Nanoparticles hybrid platinum metals - Nickel is separated from the micellar solution by centrifugation. Washed with alcohol surfactant is dispersed in water and determine the particle size as in example 1. The average particle size was equal to 19±3 nm. Particles contained 3.9% of the platinum metals, and the rest Nickel. Magnetic properties of the hybrid were investigated on the magnetometer in a magnetic field. The hysteresis curve based induction magnitno the field - induction magnetizing field showed that the particles have a super-paramagnetic properties.

Thus, the examples show that, by combining a method for concentrating ions by ion flotation or protectable to methods for producing nanoparticles of platinum and its hybrids in direct and inverse microemulsions, it is possible to obtain nano-sized particles of platinum and its hybrids with other metals from waste.

1. Method for producing nanoparticles of platinum metals, including preparation of micelles and subsequent reduction in them precursors of the metals, characterized in that for recovery use direct and inverse micelles, and before preparing micelles their concentrate from aqueous solutions by ion flotation or protectable with the use of surface-active substances (surfactants) and hydrocarbons, and after use the resulting solution of the precursor with a surfactant in the hydrocarbon to prepare micelles.

2. The method according to claim 1, characterized in that aqueous solutions using artificial mixtures of dilute aqueous solutions, waste water, poor solutions on platinum metals ores or waste solutions anode slimes electrolytic cleaning of metals.



 

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