Method of obtaining nickel (ii) oxalate dihydrate

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of obtaining nickel (II) oxalate NiC2O4·2H2O, which includes preparing of reaction water solution, which contains nickel (II), precipitation of nickel oxalate, separating of sediment from solution and its drying, in which as nickel source used are solutions of nickel chloride, nitrate, sulphate, and as reagent-precipator used is anionite AB-17-8 in oxalate form. Obtained product can be applied in industry for producing catalysts, metal films, polymetal alloys, ceramic-metal and ferromagnetic substances, as well as in production of electrovacuum devices.

EFFECT: obtaining target product of high degree of purity, which does not contain admixture anions and cations, which eliminates necessity of long washing of obtained sediment.

6 tbl, 3 ex

 

The invention relates to the field of production technology of inorganic metal compounds, in particular salts of Nickel. The resulting product can be used in industry for the production of catalysts, metal films, polymetallic alloys, metal-ceramic and ferromagnetic substances, as well as in the production of vacuum devices.

Known methods for producing oxalate of Nickel (II) Ni2O4based on the reactions of hydroxide, carbonate or soluble Nickel salts with an aqueous solution of oxalic acid followed by crystallization of the product and drying at a temperature of 100°C (Remy, the Rate of inorganic chemistry, Vol.2. - M.: Mir, 1974, s).

The disadvantage of this method is the necessity of the additional costs associated with washing of the obtained product from the impurity anions (Cl-, SO42-, and others) and cations (NH4+, Na+and others)contained in the initial solutions.

A known method of producing Nickel oxalate, comprising preparing a reaction solution containing ions of Nickel (II) and oxalate ions, the crystallization of the product, separating the precipitate from the solution (Kornienko VP // Ukrainian journal of chemistry, 1957, Volume 23, No. 2, s). The reaction solution is prepared by mixing an aqueous solution of Nickel sulfate and an aqueous solution of oxalic acid at tempera is ur 60-70°C, moreover, the reagents are mixed in an amount to provide in the reaction solution, the molar ratio of Nickel (II)oxalate, equal to 1,0:2,0. The method is based on the following reaction:

The disadvantage of this method is the necessity of the additional costs associated with cleaning product from the impurity anions and cations.

A known method of producing oxalate of Nickel (II) from spent chemical Nickel-plating solution comprising preparing a reaction of an aqueous solution containing ions of Nickel (II) and oxalate ions, the crystallization of the product from the solution, separating the precipitate from the solution and drying the precipitate (Afonin Mrs x, RF Patent №2256647, C07C 51/41, 55/07, published 20.07.2005).

The disadvantages of this method include the significant consumption of reagents (mineral acids and bases), the addition of which is necessary to maintain a given pH value in the reaction aqueous solution, the duration of the process (up to 30 days), the high temperature of its implementation, a small output and pollution of the target product. In addition, the conditions of deposition of Nickel oxalate depend on the composition of the electrolyte and require constant adjustment.

Closest to the claimed is a method for oxalate of Nickel (II), comprising preparing a reaction of an aqueous solution containing ions of Nickel (II) and OKS the lat-ion, crystallization of the desired product from the solution, separating the precipitate from the solution by filtration (Deyrieux R., Berro Ch., Puneloux A. // Bulletin de la Sociutu Chimique de France, 1973, No. 1, R). The reaction solution is prepared by mixing heated to boiling aqueous solution of salts of Nickel (II) (sulfate, nitrate or chloride) and an aqueous solution of oxalic acid.

The disadvantage of this method is the need for additional cost heating of the reaction solution and washing the product from the impurity anions and cations, as well as a low yield of the target product.

The technical result of the proposed method - obtain the desired product of high purity, containing no impurity anions (chloride, nitrate, sulfate) and cations (sodium, potassium), which eliminates the need for long-term leaching of the resulting sludge. When creating the claimed invention, the aim was to develop an ion-exchange method of producing oxalate of Nickel (II). This task includes the selection of annita, translation of anionite AV-17-8 (strong-base anion exchange resin with a polystyrene matrix containing Quaternary ammonium base - N+(CH3)3(GOST 20301-74)) in the oxalate form, the contact of the resin with a salt solution of Ni (II), Department of product and regeneration of the anion exchange resin. New this method is that as reagent-precipitator using anion oxalate in the Orme and therefore the product is not contaminated by the cations of the precipitator and the anions of the solution.

When a claimed invention were used gel and porous weakly basic and strong-base anion exchange resin in C2O4-form. The findings suggest that the use of porous (weakly basic and strongly dissociated), and gel weakly basic anion exchange resin is impractical because a significant proportion of Nickel (>50%) is retained by the anion exchange resin due to its deposition in the form of oxalate of Nickel (II) in the pores of the sorbent or complexing ions of Nickel (II) with nitrogen functional groups. Therefore, the choice of strong-base anion exchanger containing functional group Quaternary ammonium bases of the type AB-17-8 or analogues, is preferred.

The translation of the anion in C2O4form held, filling the original AV-17-8 in the chloride form 3 times a 1.8 m solution of K2C2O4(m:f=1:3), allowing each portion of the solution within one hour (the last portion - within days). Then the resin was washed with water to the lack of analytical reactions to the oxalate ion with 1M SrCl2(the limit of sensitivity reactions 10-5M). The resulting resin was dried at a temperature of about 60°C and after determining the content of oxalate ions were used in experiments.

The process can be described by the following equation:

.

(Superscript feature definition is employed, the phase anion-exchange).

The mass of the anion (m) for synthesis was calculated by the formula

,

where CPIAPthe concentration of the original solution of Nickel (mmol/ml), VNi- volume of a solution of Nickel (ml), WITH the content of oxalate ions in the anion exchange resin, mmol-EQ·g-1.

A portion of the anion exchange resin was brought into contact with 10 ml of salt solution of Ni (II) concentration was varied in the range 0.1-0.5 M) at a fixed temperature for a certain time while mixing on a shaker. The phases were separated, passing them sequentially through a sieve with a diameter of holes of 0.25 mm (for the Department of anion exchange resin and filter "blue ribbon" or by centrifugation (precipitate). Further, the anion exchange resin was washed with water from the precipitate. The washing water was collected and determined the concentration and the amount of Nickel in them and in the contact solution.

Sediment Ni2About4·2H2After washing with water, was dried at a temperature of 60-80°C. the Anion exchange resin after synthesis of the salt of Nickel (II) was washed with 10 ml 1M NGO3when mixing on a shaker for one hour. The procedure was repeated three times, the resulting solutions were collected in a flask of 50 ml, was brought to the mark with distilled water and determined the amount of Nickel in aqueous solution.

Then counted the molar fraction of Nickel by the equation

,

where nCothe amount of Nickel in the analyzed phase (mmol), n0 Co- the total amount of Nickel in the system (mmol), b is the molar fraction of Nickel (%).

Below are examples of the proposed method.

Example 1. Getting oxalate of Nickel from sulfate solution Nickel. To 10 ml of a 0.35 M solution with NISO4add the anionite AV-17-8 in oxalate form. The solution is stirred for 15 min on a shaker at a temperature of (20±1)°C, then the phases are separated, determine the molar fraction of Ni(b) in different phases (ion exchange, precipitation, contact solution, washing water). The data obtained as the average of 3 parallel experiments are shown in table 1.

Table 1
The distribution of Nickel (b) phase
b(Ni) phases, %
contact solutionsedimentIonithlavage
4,858,433,63,2

The precipitate was analyzed by thermogravimetry, complexometry and permanganate. In the sediment is not detected anions original Nickel salts within the sensitivity of the qualitative reactions. The results are presented in table 2. Output 58,4%.

Table 2
Elemental composition (ω - mass fraction) of the obtained product
ω (Ni2+), %ω (C2O42-), %ω (H2O)%
calculationfoundcalculationfoundcalculationfound
32,2of 31.848,147,719,720,6

From the data of table 2 shows that the composition of the product corresponds to the formula NiC2O4·2H2O.

Example 2. Getting oxalate of Nickel nitrate solution of Nickel. To 10 ml of a 0.35 M solution of Ni(NO3)2add the anionite AV-17-8 in oxalate form. The solution is stirred for 15 min on a shaker at a temperature of (20±1)°C, then the phases are separated, determine the molar fraction of Ni(b) in different phases (ion exchange, precipitation, contact solution, washing water). The data obtained as the average of 3 parallel experiments are shown in table 3.

Tab the Itza 3
The distribution of Nickel (b) phase
b(Ni) phases, %
contact solutionsedimentIonithlavage
4,665,626,92,9

The precipitate was analyzed by complexometry and permanganate. In the sediment is not detected anions original Nickel salts within the sensitivity of the qualitative reactions. The results are presented in table 4. Output 65,6%.

Table 4
Elemental composition (ω) of the obtained product
ω (Ni2+), %ω (C2O42-), %ω (H2O)%
calculationfoundcalculationfoundcalculationfound
32,2of 31.848,148,419,8

From the data of table 4 shows that the composition of the product corresponds to the formula NiC2O4·2H2O.

Example 3. Getting oxalate of Nickel chloride solution of Nickel. To 10 ml of a 0.35 M solution of NiCl2add the anionite AV-17-8 oxalate form. The solution is stirred for 15 min on a shaker at a temperature of (20±1)°C, then the phases are separated, determine the molar fraction of Ni(b) in different phases (ion exchange, precipitation, contact solution, washing water). The data obtained as the average of 3 parallel experiments are shown in table 5.

Table 5
The distribution of Nickel (b) phase
b(Ni) phases, %
contact solutionsedimentIonithlavage
the 3.865,427,63,2

The precipitate was analyzed by complexometry and permanganate. In the sediment is not detected anions original Nickel salts within the sensitivity of the qualitative reactions. The results are presented in table 6. The yield of 65.4%.

Table 6
Elemental composition (ω) of the obtained product
ω (Ni2+), %ω (C2O42-), %ω (H2O)%
calculationfoundcalculationfoundcalculationfound
32,231,648,147,619,720,8

From the data of table 4 shows that the composition of the product corresponds to the formula NiC2O4·2H2O.

The proposed method is quite simple, does not require the use of aggressive media, high temperatures and pressures. Using it, you can obtain a product of high purity, containing no impurity anions (chloride, nitrate, sulfate) and cations (sodium, potassium), which means in the future need long-term leaching of the resulting sludge.

The method of producing oxalate of Nickel (II) NiC2O4·2H2O, comprising preparing a reaction of an aqueous solution containing Nickel(II), OSA is giving oxalate of Nickel, separating the precipitate from the solution and drying, characterized in that as the source of Nickel use solutions of the chloride, nitrate, Nickel sulfate, and the reagent-precipitator using anion exchange resin AV-17-8 in oxalate form.



 

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3 cl, 1 tbl, 3 ex

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2 cl, 1 tbl, 1 ex

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5 cl, 1 tbl, 14 ex

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2 cl, 1 tbl, 8 ex

FIELD: chemistry.

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1 tbl, 10 ex

FIELD: organic chemistry, chemical technology, agriculture.

SUBSTANCE: invention relates to a method for preparing the preparation comprising triterpenic acid water-soluble salts and additionally added protein-containing product and vegetable raw, the source of triterpenic acids taken in the following ratio of components, wt.-%: protein-containing product, 10-17; triterpenic acid sodium salts, 4-5, and vegetable raw, the balance. Method involves mixing triterpenic acid-containing vegetable raw with the protein-containing product taken in the ratio = (9-11):(1-2), mechanical-chemical treatment of this mixture in activator device, mixing of prepared semi-finished product with sodium carbonate or sodium hydrocarbonate taken in the ratio = (92-97):(3.5-8.3) and repeated treatment in the activator device. Method involves applying flow-type ball vibration-centrifugal or ellipse-centrifugal mills as the activator device that provide the acceleration of milling bodies up to 170-250 m/c2 and time for treatment for 1.5-3 min. Invention provides simplifying the process and the complex processing waste in lumber industry.

EFFECT: improved preparing method.

6 cl, 1 tbl, 6 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing copper (II) acetate monohydrate that represents organic carboxylic acid salt. Copper (II) acetate monohydrate is prepared by crystallization from solution obtained by mixing acetic acid, alkaline metal acetates or ammonium with copper-containing spent solution used in etching printing boards. Method provides reducing cost of the proposed method for preparing copper (II) acetate monohydrate, retaining purity of product with simultaneous utilization of toxic waste in electronic engineering manufacture - the spent solution in etching printing boards. Also, invention provides reducing material consumptions in preparing copper (II) acetate monohydrate, expanding assortment of materials used for its preparing and utilization of toxic waste in electronic engineering manufacture. Product obtained by the proposed method can be used as pigment, fungicide and copper microfertilizer in agriculture, as catalyst in processes of polymerization, as a stabilizing agent of artificial fibers, for preparing galvanic solutions and preparing other copper compounds.

EFFECT: improved preparing method.

14 cl, 5 ex

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