SU1527169A1 - Method of producing nickel carbonyl - Google Patents

Abstract

The invention relates to carbonyl technology and allows obtaining carbonyl nickel of high purity by treating sintered nickel powder with a bulk porosity of 20–70% by volume and a specific surface area of 0.3–0.7 m ² / g with carbon monoxide containing 0.1–0. , 3% by volume of oxygen. 1 tab.

Description

(21) 426983А / 23-26

(22) 05.22.87

(46) 12/07/89, Bull. Number 45

(72) B.YA, Dyer, V.I. “Bader,

Yu.I. Gubernsky, AoS. Mnukhin,

V.O.Akop n, F.A.Goloshchapov

and A.Fosdvizhkov

(53) 661,874 (088.8)

(56) USSR author's certificate

 260626, cl. Since 01 G 53/02, 1970.

(54) METHOD FOR MAKING A NICKEL CARBONIP

(57) The invention relates to carbonyl technology and makes it possible to obtain high purity nickel carbonate by treating sintered nickel powder with a volume porosity of 20-70%, and a specific surface area of 0.3-0.7 m / g carbon monoxide containing 0.1 -0.3% by volume of oxygen. 1 tabl,

The invention relates to the field of carbonyl technology and can be used in the production of highly pure nickel carbonyl for the application of protective nickel coatings on energy equipment.

The purpose of the invention is to improve the purity of the carbonyl nickel.

Carbonyl nickel with a bulk porosity of 20–70 vol.% And a specific surface area of 0.3–0.7 is taken as the starting material for carbonyl dop synthesis of carbonyl powder and treated with carbon monoxide containing 0.1–0.3% by volume. % oxygen

The presence in the reaction gas of 0.1–0.3% oxygen contributes to the oxidation of trace elements with high means to an electron, in particular iron, and their transition to a noncarbonylated state, since the transition metals of the iron group in the oxidized state are not carbonylir - are. It is the presence of oxygen in the reaction gas, along with a large metal-gas interface for

the expense of the porous structure of the source material provides a deeper purification from iron micronutrient nickel carbonyl already at the stage of synthesis. When the oxygen content in the reaction gas is less than 0.1 vol.%, No significant iron removal is observed at the synthesis stage. Oxygen content: in a gas of 0.3% by volume, it is unreasonable for safety,

Carbonylation of a material with a porosity of less than 20 vol.% And a specific surface area of less than 0.3 is impractical, since the purity of the nickel carboxyl and the intensity of the carbonylation process are reduced by reducing the metal-gas interface. The use of sintered nickel with a porosity above 70 o6.Z and a specific surface area above 0.7 MVr is impractical for two reasons. First, carbonylirovanie material with such a developed surface leads to a difficult to control development of the synthesis reaction, which makes it difficult to maintain

(L

with

YU

M

Od

technological process and contributes to the transition into the carbonyl phase of undesirable impurities. Secondly, this material is characterized by low strength properties, easily destroyed, which leads to a large amount of dust removal and makes it difficult to shape the process.

Example. PNA carbonyl nickel powder is sintered in a neutral atmosphere at 400 ° C for 2 hours. The resulting briquettes of porous nickel containing 0, 18 wt.% Iron are processed with carbon monoxide with different oxygen content at a pressure of 25 MPa and a temperature in the reactor of 220 ° C. Carbonyl undergoes termination of such dissociation in the decomposer and the iron content in the final - nom metal.

The iron content in nickel obtained from a carbon type synthesized from sintered nickel powder by treatment with carbon monoxide containing oxygen is given in the table.

The content of carbonyl iron impurity in nickel carbonyl is, according to the known method, 0.0017-0.0022 vol.%

As can be seen from the above data, the introduction of oxygen in the amount of 0.1–0.3 vol.% In the reaction gas and the use of porous sintered carbonyl nickel as the starting material for carbonylation of the material makes it possible to reduce the iron content in the final

Oxygen content in the reaction gas,

about. 20.06 0.10 0.16 0.22 0.27 0.30 0.34

Sintered nickel porosity,

about. Z16 20 33 49 58 70 75

Specific over

Q

five

the metal is below 0.001 w / o, and when the oxygen content in the gas is at a level of 0.25% by volume and the porosity of the sintered material is 50-60%, the iron impurity in the final metal is 0.0005- 0.0006% by weight.

Carrying out the synthesis of carbonyl nickel from nickel powder according to the proposed method in comparison with the known method shows that 30-50% of iron contained in the initial powder passes into the carbonyl phase. When the PNA nickel powder containing 0.0018% by weight of iron is treated by this method, the concentration of iron in nickel obtained as a result of the association of carbonyl synthesized from powder is 0.0005-0.0009% by weight, thereby the carbonate quality increases to 2-3 times.

Claims (1)

Invention Formula The method of producing nickel carbonyl by treating carbon with carbon dioxide with highly dispersed nickel powder at a twisted temperature, characterized in that, in order to increase the purity of the target product, fine nickel powder is sintered to obtain particles with a porosity of 20-70% by volume and a specific surface of 0.3-0, 7 m / g and treated with carbon monoxide containing 0.1-0.3% by volume of oxygen.