SU1689305A1 - Method of producing analysis grade purity nickel (ii) nitrate-6-water free of cobalt - Google Patents

Abstract

This invention relates to the preparation of high-purity nickel salts and can be used in analytical chemistry and electroplating. The purpose of the invention is to intensify the process by accelerating the separation of impurities and eliminating the stage of evaporation of an aqueous solution of the target product. An aqueous solution of the original nickel nitrate containing 280-350 g / l is treated with a reagent. As a reagent, isododecylphosphonate acid, dissolved in an organic solvent which is not miscible with water, and treated with nickel hydroxide, taken in the calculation of 0.02-0.04 r-eq of OH ions per 1 g-eq of M 2 + ions, is used as a reagent. the ratio of aqueous and organic solutions, equal to 1: (0.02-0.2). The impurities are transferred to the organic solution and with it are separated from the aqueous solution of the target product. From the latter, Ni (N03) 2 6H20 is crystallized. The process of separating impurities in comparison with the prototype is accelerated by 8-9 times. 2 tab. SP

Description

This invention relates to the production of high-purity nickel salts and can be used in analytical practice, electroplating, etc.

The purpose of the invention is to intensify the process by accelerating the separation of impurities and eliminating the stage of evaporation of an aqueous solution of the target product.

To obtain Ni (N03) -6H20 chDA without Co, an aqueous solution of technical nickel nitrate is prepared with a nickel ion content of 280-350 g / l. The solution is treated with a reagent. Isododecylphosphetanic acid (IDDPC), dissolved in a water-immiscible organic solvent and treated with nickel hydroxide, calculated as 0.02-0.04 r-equiv. Of OH-ions per 1 g-eq of M 2 + -ions, is used as a reagent. , at a volume ratio of aqueous and organic solutions, equal to 1: (0.02-0.2). The impurities are transferred to the organic solution and with it are separated from the aqueous solution of the desired product. From the latter, M (MO3) 2.6H20 is crystallized.

Ensuring the high purity of the target product is due to the ability of IDDFC to interact with metal ions that contaminate the initial nickel nitrate:

About 00 YO

about

SP

Me2 ++ 2 H Rz MeR2 + 2 H.

Well oj. Oa.

where Me5 + -C02 +, Zn2 + HR-IDDFC;

Fe2 +. Cu

2+.

0)

CM CI SI

 N

si

2 +

DROPPED

about

11 cm cm ions N IDD1 -, - fi 1 adherent amount, the introduction of CHf ions is necessary for shifting the equilibrium of the reaction H) to the right and provides for the formation of a low dissociation of the H20 compound and the syrup of IDDFC with metapps.

Changing the volume ratio of water and opi of the epic solution in the direction of reducing the organic phase and introducing ions less than the indicated amount ensures the required quality of the product. Increasing the number of e ions is not practical from an economic point of view. Optimal concentration f in the i / l solution. At a concentration of NI, a pH of 240 g / l and below, to obtain a nitrateg crystalline hydrate. Nickel is required to supplement the evaporation of the solution, and after the concentration of nickel is more than 30 g / l, the crystallization process begins during filtration, resulting in loss of product.

Example 1 In a glass reactor, 100 ml of an aqueous solution of nickel nitrate with an NI concentration of 300 g / l are placed and 0 ml of a 25% -noiO solution of IDDFC in toluene, nfjpaf and cast 1.4 g of N1 (04) 2 are added. The mixture is heated to 65 ° 70 EEG, stirred for 10 minutes, leave it n. U) min, then the solution; JifN03} 2 separated from the organ. The physical phase and crystallize. The yield of this mixture is 84 5% Söder of the mixture in crises, the allohydrate is% Cn 0.00035, 1l 0 0008, Guy S00i4 Fe0 0004.

The methods of performing other examples according to the invention are similar. The conditions of the process and the nature of the product are given in table. one.

Compared with prototyg, the invention speeds up the process of purifying the initial technical nickel nitrate. Comparison of methods for producing Ni (NO)) 2.6X20 ChDA without Co according to the invention

and the prototype is shown in Table 2. It follows from the presented data that the invention speeds up the process of purification of nickel nitrate by 8-9 times. In addition, the invention allows to reduce energy consumption

by using a concentrated solution of the starting nickel nitrate and eliminating the step of preparing the purified solution.

Claims (1)

Invention Formula A method of producing nickel nitrate of six-day-grade ChDA grade without cobalt, including treating an aqueous solution of the initial nickel nitrate with a reagent, separating g remittances and crystallizing the target i lz of its aqueous solution, characterized in that, in order to intensify the process by accelerating the stage of removing impurities and eliminating the stage of evaporation of an aqueous solution of the target product., a solution containing 280-350 is used as an aqueous solution of nickel nitrate g / l of nickel ions, and isododecyl phosphate is used as a reagent | ethanoic acid dissolved in non can be mixed with water, organic res-gvoriotepe and treated with nickel hydroxide taken in the calculation of C, 02 0.04 g-eq g of hydroxide ions of I-gcpp of nchke 1P ions, PrI Oba. MIOM rOOrHOLUJHHH WATER AND organic r tsor equal to 1: (0,020 2) h and c a 1 Continued table. one n, OGOS and, P005 OLSiB Ninel nitrate B-water we Co NP /, GOST 4i5e-73 (with changes) T and o l g c l 2 . “., frjTQTMn (pic, uH paLiHP NiZf in ishpd-B; 1.7  PRESTATOR, Stages of the process, Osan dvnii priisp1, t pe-iH2 I Chdchlnsnm psprt Upogivvnie rrt-vsra, --Ch 1 hp.ic i a g dip 1, and t tp m -i  o melemts-1 suspension- separation of suzpsznash type Sr | -t prsa / nta with ONE unit, ig / l0,136 PED / Agzomy  AO-353 Ivniee poig: skgi, 2G min FROM ALLRUPT FRI TGRANICAL FIH, 10 pin Chapistallis ui 0.196-0.545