Method of producing ultramicrodispersed nickel oxide powder using ac

FIELD: electricity.

SUBSTANCE: method of producing ultramicrodispersed nickel oxide powder includes electrolysis in 17 M sodium hydroxide solution under alternating sinusoidal current at 20Hz with nickel electrodes. The process of electrolysis is carried out at temperature of 20-30°C and voltage across the electrodes of 4V.

EFFECT: method for producing ultramicrodispersed nickel oxide powder suitable for use in catalytic production of nanocarbon materials by pyrolysis of hydrocarbons while reducing heating costs and simplifying its cell structure.

3 ex

 

The invention relates to methods for producing powders of metal oxides, and in particular to methods of obtaining ultramicrobacteria powder of Nickel oxide. The resulting powder can be used to prepare the catalysts used in the synthesis of carbon nanotubes.

There are different ways of obtaining ultramicrobacteria particles of Nickel and its oxides. They can be divided into three large groups: chemical, physical and physico-chemical methods.

1. Chemical methods

These include vapor deposition, recovery in solid and liquid phase pyrolysis, Sol-gel technology.

Method for the synthesis of nanosized particles of Nickel oxide is in the deposition of nitric acid solution in ethanol medium (ethanol, propanol), a diluted solution of sodium hydroxide at a temperature of 60...80°C, followed by washing precipitation with water, and drying at 50°C. the Obtained hydrated oxides of Nickel NiO·nH2O have a specific surface area of 280 mg/cm2[L.N. Trushnikova, V.V. Sokolov, V.V. Bukovec. Obtaining nanosized particles of oxides of cerium, copper, cobalt and Nickel // the Second all-Russian conference on nanomaterials, "Nano-2007". 13-16 March 2007. Novosibirsk. S]. One of the problems of receiving such materials from aqueous solutions is the agglomeration of ultram the nkiye particles. To prevent clumping use organic liquids, including alcohol. This expensive and inefficient method finds application in laboratories and for special purposes.

There is a method for the synthesis of nanosized powder of Nickel oxide deposition from solution and in which as initial reagents used nitrate of Nickel, and the precipitant is ammonium carbonate [A.G. Belous, AS Yanchevskii, ALEXANDER Kramarenko. Getting nanomateriales oxides of Nickel and cobalt from solutions // Journal of applied chemistry, 2006, №3. S.353-357]. Formed during thermal decomposition of basic carbonate particles of Nickel oxide have a rounded shape with particle sizes of 5-10 nm.

Nanoparticles of Nickel synthesize traditionally-chemical method in reverse micelles [SV Gornostaeva, A.A. Revin. Synthesis and properties of nano-size particles of Nickel and nanocomposites // physical chemistry of surfaces and protection of materials. 2008. No. 4. S.400-403]. To prepare the solution using hydrated nitrate Nickel and trichitillomania water. To obtain reverse micelles as a surface-active composition used a solution of bis(2-ethylhexyl) and sulfosuccinate sodium in isooctane. Adsorption of nanoparticles of Nickel is carried out on silochrome. The prepared solution is irradiated on the installation RKHM-γ-20 (source60/sup> Co). Absorption of radiation dose on ferrosulfate the dosimeter equal 0,26 G/C. Zlecenia dose - of 17.8 kGy. The resulting Nickel nanoparticles have a spherical shape and sizes of the order of 1 to 100 nm. Found that the oxygen of the metallic Nickel particles are oxidized to nanoparticles of Nickel oxide (II).

Method for obtaining nanosized particles of Nickel oxide chemical recovery from aqueous solutions of salts of Nickel [A.L. Novozhilov, GV Narseev, L.V. Serov. Obtaining nanoparticles of Nickel // VII international conference. Moscow - Stavropol: Sevkat, 2007. - 510]. As a stabilizer using 1% aqueous solution of polyvinyl alcohol as a reducing agent used sodium borohydride. The concentration of Nickel sulfate range from 0.1 to 0.001 mol/DM3, sodium borohydride is from 1.0 to 0.01 mol/DM3. The resulting suspension is very stable and remain in suspension for more than a week. The sizes of the particles in this solution, have an average radius of 280 nm, with a large asymmetry of the distribution curve in the direction of increasing particle size.

The Nickel powder is produced by recovery from solutions of salts of Nickel, elemental phosphorus, taken in its active form in an alkaline environment, and before recovery to the original solution injected silicone grease [A.S. No. 1479539, to the. SI 23/04, 16.03.87, publ. 15.05.89]. The resulting powders have a high ferromagnetic properties, and low bulk weight.

A known method of extraction of the Nickel powder from waste solutions chemical Nickel plating, including his recovery from solutions by hypophosphite sodium, characterized in that to reduce the content of Nickel ions in the solution to the maximum permissible concentrations in the waste electroplating plants recovery of Nickel is carried out in the presence of the Nickel powder at a pH of 6.5...7,0, temperatures 65...70°C, and the ratio of the content of Nickel ions and hypophosphite sodium 1:5 [A.S. No. 1673616, CL C22B 3//44,C22B23/00, 31.05.89, publ. 30.08.91].

Known methods for producing the Nickel powder by restoring its salts with hydrogen by the method [Application Germany No. 2244746, CL C22B 23/04, publ. 10.07.75] solution douglasthe Nickel is treated with gaseous ammonia or aqueous ammonia solution, the precipitate Ni(NH3)6Cl2separated by filtration, dried to a partial transformation in Ni(NH3)2Cl2and restore at 450...1000°C hydrogen; by the way [France Application No. 2227336, CL C22B23/04, B22A 9/00, publ. 27.12.75] the source of Nickel salt solution is treated with alkali metal oxalate, restore the sediment in the autoclave with hydrogen in the presence of a hydroxide of an alkali metal.

Method for obtaining Nickel powder by hydrogen deposition in an autoclave at elevated temperature and pressure [A.S. No. 1126374, CL B22F 9/24, C22B23/04, 18.05.82. publ. 30.11.84]. With the aim of increasing the activity of powder and cheaper process, the deposition of lead from aqueous slurry of Nickel carbonate with the addition of sulfate ion in the amount equivalent to 0.05 mol of Nickel per 1 mol of Nickel carbonate, and after deposition of the slurry is injected inhibitor with restorative properties. As an inhibitor use formic acid in the amount of 0.5 to 2 g per 1 DM3slurry of Nickel powder.

2. Physical methods

These include techniques based on the processes of evaporation and condensation. The powders are formed as a result of the phase transition of vapor - solid or vapor - solid - liquid in the gas volume or on the surface to be cooled.

Developed a new process of manufacturing a Nickel nano-powder in an atmosphere of various gases (air, argon, nitrogen, helium, xenon. The process is the evaporation of solid natural or technogenic raw materials, followed by rapid cooling of high-temperature steam and condensation of matter in the form of nanoparticles [S. p. Bardachanov, A. I. Korchagin, NICHOLAS Kuksov, A. Lavrukhin, R.A. Salimov, S.N. Fadeev, V.V. Shards. Getting managesearch powders on a powerful mustache is oritel electrons at atmospheric conditions // Laurentian reading, mathematics, mechanics and physics. Novosibirsk, 27-31 may, 2005 http://www.ict.nsc.m/ws/show_abstract.dhtml?ru+120+66]. The latter can have different sizes from 10 to 500 of them. The process provides a temperature sufficient to vaporize any material at the heating temperature of more than 1000 K/s Additional advantage is fewer production stages.

Obtaining a powder of Nickel oxide is also an electric explosion of Nickel wire with different diameters and length [Y.A Kotov, A.V. Bagazeev, IV Beketov. Characterization of powders of Nickel oxide obtained by electrical explosion of wire // Journal of technical physics. 2005, volume 75, issue 10. P.39-41.]. Apply discharge circuit with an inductance of 0.5 μh, and the capacitance of the capacitor Bank 3,2 international film festival. Charging voltage change from 10 to 33 kV. The explosion is carried out at normal pressure in a mixture of nitrogen and oxygen and the change in concentrations of from 10 to 30%. The resulting particles have different shapes both monocrystalline and polycrystalline structure with a particle size of about 100 nm.

3. Physico-chemical methods

These include the processes of evaporation - condensation involving chemical reactions, electro-deposition, drying - freezing.

Ultramicrobacteria powder of Nickel oxide can be obtained by the method of freeze-drying [Roehrig F.K., Wright .R. Freeze drying: a unigue aproach to the synthesis of ultrafme powders. - J. Vac. Sci. and Techn., 1972. 9. No. 6. P.1368-1372]. Of raw materials, in particular metal salts, prepare a solution of the required composition, which quickly freezes by spraying into the chamber with a cryogenic environment (e.g., liquid nitrogen). Then the pressure of the gaseous medium above the frozen granules is reduced so that it was below the equilibrium point formed by the cooling system, and the material is heated in a vacuum to the sublimation of the solvent. The resulting product consists of a very thin porous granules of the same composition. Further processing depends on the purpose of the final powder. Calcination of the pellets in the air, you can get the oxides of Nickel, recovery powder suitable metal.

The Nickel powder is produced by electrolysis of ammonium sulfate solutions of Nickel (the source material is with NISO4·7H2O). The electrolyte contains 5...15 g/DM3Nickel (Ni % 75...80 g/DM3ammonium sulfate, 2...3 g/DM3sulfuric acid, 40...50 g/DM3ammonium chloride and 200 g/DM3sodium chloride. The electrolysis is conducted at the temperature of the electrolyte 35...55°C, current density of 1000...3000 a/m2and the voltage on the tub 10...15 Century, the current Output is up to 90...94%, and the power consumption of about 3000 kWh/t [Libenson GA Fundamentals of powder metallurgy. M: Metallurgy. 1975. s].

The described process is perceived by the Oia powders of oxides of Nickel by electrolysis on a symmetric alternating current (50 Hz), according to which the maximum rate of destruction of the Nickel - 20 mg/(cm2·h) was observed in 46% sodium hydroxide solution at current density of 2.5 a/cm, the electrolyte temperature 70°C [V.V. Korobkin. The destruction of Nickel and cadmium in the electrolysis of alternating current of industrial frequency // Bulletin of the Tomsk Polytechnic University. 2003. No. 1. P.23-24].

The closest in technical essence and the resulting effect to the claimed method is a method of obtaining Nickel oxide, described in [EJ Nikiforova and other "Development of an electrochemical method of producing ultramicrobacteria powder of Nickel oxide by electrolysis in an alternating sinusoidal current". Proceedings of the II all-Russian scientific-innovative youth conference with international participation "Modern solid state technology: theory, practice and innovation management". - Moscow: Publishing house of the GOU VPO TSTU, 2010. - S-237] (prototype). The method is carried out in a thermostatted cell 17 M solution of sodium hydroxide at a current frequency of 20 Hz and the voltage on the electrodes 4 Century. a Constant solution temperature of 70°C in a cell support with the help of a thermostat with an accuracy of 0.5°C.

Our proposed method of obtaining ultramicrobacteria powder of Nickel oxide on an alternating sinusoidal current with Nickel electrodes is 17 M solution of hydro is sid sodium, when the current frequency of 20 Hz, a temperature of 20-30°C and a voltage of 4 C. the Rate of destruction of the Nickel electrodes (education ultramicrobacteria powder of Nickel oxide) is not reduced in comparison with the prototype.

The method is as follows.

The electrolysis is performed on an alternating sinusoidal current at the Nickel electrode, the cell volume of 200 cm3at a current density of 2.5 a/cm2, frequency current of 20 Hz and a temperature of 20-30°C, when the voltage at the electrodes 4 C. the Electrode and thermometer fixed in the insulating cover, for example, PTFE or polypropylene. After a predetermined time process, the electrodes are removed from the cell, washed with distilled water and alcohol, and then weighed on an analytical balance. The resulting powder was separated by filtration, washed with distilled water, dried and weighed. The rate of destruction of Nickel and education ultramicrobacteria powder of Nickel oxide determined by the gravimetric method.

A distinctive feature of the proposed method is:

is that the electrolysis process is carried out at a temperature of 20-30°C and the voltage on the electrodes 4 Century

The proposed method of obtaining powder of Nickel oxide is illustrated by the following examples:

Example 1

Electrolysis 17 M sodium hydroxide solution with an alternating current spending is in the electrochemical cell the Nickel electrodes. The temperature of the starting solution is 20°C, the voltage at the electrodes is 4 Century, the Rate of destruction of Nickel determined by the gravimetric method. The surface speed of the destruction of Nickel is 75 mg/(cm2·h).

Example 2

Electrolysis 17 M sodium hydroxide solution, with an alternating current, is carried out in the electrochemical cell the Nickel electrodes. The temperature of the starting solution is 25°C, the voltage on the electrodes is 4 Century, the Rate of destruction of Nickel determined by the gravimetric method. The surface speed of the destruction of Nickel is 75 mg/(cm2·h).

Example 3

Electrolysis 17 M sodium hydroxide solution, with an alternating current, is carried out in the electrochemical cell the Nickel electrodes. The temperature of the starting solution is 30°C, the voltage at the electrodes is 4 Century, the Rate of destruction of Nickel determined by the gravimetric method. The surface speed of the destruction of Nickel is 75 mg/(cm2·h).

The method of obtaining ultramicrobacteria powder of Nickel oxide in 17 M solution of sodium hydroxide by electrolysis of an alternating sinusoidal current with frequency of 20 Hz with Nickel electrodes, characterized in that the electrolysis process is carried out at a temperature of 20-30°C and the voltage on the electrodes 4 Century



 

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