The way hydroxide nickel (ii)

 

(57) Abstract:

The invention relates to the field of producing compounds of Nickel, in particular to technology hydroxide Nickel (II) used for current sources, for example, in the composition of the active mass of the positive electrodes of alkaline batteries. The invention consists in the method of producing Nickel hydroxide (II) for current sources, including the preparation of the initial solution of the hydroxide of alkali metal salt of Nickel (II) and barium hydroxide, mixing them, the precipitation of the hydroxide of Nickel (II) separating the mother liquor, sludge treatment with alkali in an autoclave at a temperature of 130-200oWith, washing the precipitate and drying. The alkali treatment is carried out at the concentration of hydroxyl ions in the liquid phase of the pulp, 0.05-0.3 g-ion/liter Washing of the precipitate is carried out in three stages: the first stage of water in the second stage with a solution of barium hydroxide with a concentration of 2-6% and in an amount to provide a mass ratio of the solution to precipitate (1-2):1, and in the third stage, again with water. The method is simple, eliminates the time-consuming and energy-intensive operation of the sludge drying before washing. The product reduces the content of water-soluble impurities anions SO42-Cl-. 2 C.p. STI to technology hydroxide Nickel (II), used for current sources, for example, in the composition of the active mass of the positive electrodes of alkaline batteries.

Prior art

The known method hydroxide Nickel (II) used for alkaline batteries (M. A. Dalian, Century Century novoderezhkin and F. F. Tomaszewski "Manufacture of electric accumulators", M., "Higher school", 1977, pp. 260-277). The method involves the preparation of initial solutions of sodium hydroxide, sulfate Nickel (II) and barium hydroxide as adjuvants and the mixture of them. The precipitate is separated by filtration, then is subjected to the first drying, washing from sulfate ions, the second drying and grinding. The disadvantages of the method are its duration and large energy costs associated with the need to double-dried product obtained.

A method of obtaining Nickel (II) hydroxide, which includes the injection of a solution of Nickel sulphate in alkaline solution, ochiltree and drying the precipitate, washing from sodium sulfate, re-drying, treatment with alkali boiling, washing with water and final drying (ed. mon. SU 51380, 1937). Three drying makes the process very long and labor - intensive.

Famous t is yuusei Supplement containing barium ions. This is followed by precipitation, separation of the mother liquor, centrifuge sludge is first dried to a certain moisture, washing away impurities and the second drying. After first drying the resulting paste is injected with a solution containing ions of cobalt (patent RU N 2138447). The method has the same drawbacks as in the previous case. In particular, each of the two stages of drying lasts about 24 hours.

The invention

The proposed method significantly reduces the duration of the process and reduce the cost of obtaining hydroxide Nickel (II) with a simultaneous increase of its quality.

The way hydroxide Nickel (II) current sources includes the preparation of the initial solution of the hydroxide of alkali metal salt of Nickel (II) and barium hydroxide (adjuvants), mixing them, sedimentation and separation of the mother liquor, subsequent washing of the precipitate and drying. When this residue before washing processed with alkali in an autoclave (hydrothermal treatment). The treatment is carried out at T=130-200oC, maintaining the concentration of hydroxyl ions in the liquid phase of the pulp 0.1-0.5 g-ion/liter

Washing the precipitate preferably conducted in three stages: the first stage of water in the second stage solution and in the third stage, again with water.

In the first stage of washing separates the main mass of the soluble salts, the impurity metals in the second stage, additional extraction in solid phase remaining in the liquid phase in the pores of the sediment sulfate ions due to the formation of low-solubility of barium sulfate in the third stage - goatmilk sludge from cations of barium and soluble salts.

The positive effect of hydrothermal processing on the proposed method is called with the result of this processing by changing the composition and structure of the sediment and the resulting properties (specific volume, the electrochemical capacity, the content of impurity anions included in the structure of the sediment in the form of basic sulfates of the type (3-6)Ni(OH)2With NISO4and the basic chloride of type (1-3)Ni(OH)2NiCl2and also in the form of soluble sulfates and chlorides, adsorbed to sediment). Presumably, this change occurs by the following mechanisms: the ordering patterns of sediment (transition from x-ray amorphous state to crystalline), collective recrystalization and dehydration emitting adsorbed salts and water and basic hydrolysis of salts emitting structural sulfate and chloride ions in the liquid phase.

the ü the content of water-soluble impurities anions SO42-and Cl-in the hydroxide Ni (II) and its specific volume, and improve the electrochemical capacity of the product. In addition, obtaining hydroxide Ni (II), according to the invention, reduces the technological process by eliminating the operation of drying before washing the hydroxide precipitate Ni (II) from impurities.

Information confirming the possibility of carrying out the invention

For the deposition of Nickel hydroxide (II) the known methods has prepared the following solutions:

the sodium hydroxide solution with a concentration of 26.5%, the specific gravity of the solution 1295 kg/m3at T=15oC;

a solution of Nickel sulfate (II) with a concentration of 15.5%, the specific gravity of the solution 1175 kg/m3at T=15oC;

a solution of barium hydroxide (activator) with a concentration of 4%, the specific gravity of a solution of 1100 kg/m3at T=70oC.

In a reactor with a capacity of 1.2 m3equipped with a mechanical stirrer and a heater, poured the prepared solution of sodium hydroxide in a volume of 150 liters and heated to 50oC. Then with stirring for 1 hour the reactor was simultaneously filed a pre-warmed to 50oC solution of Nickel sulfate and 75oC solution of barium hydroxide in quantities 460 l and 25 l of sootvetsvenno and determined the content of sodium hydroxide in the liquid phase, which must be at the level of 4-10 g/l In these conditions the deposition it was 6.2 g/L.

After the deposition of the slurry with a temperature of 60oC sent to the filtering centrifuge, in which the separated mother liquor from the precipitate. Pressed on the centrifuge sludge with a moisture content of 15-20% was collected in tank reulator V=1 m3where filed an aqueous solution of sodium hydroxide with a concentration of 0.2 g-EQ/l to establish the ratio of T:W=1:(5-6). After stirring for 10 minutes, took away the pulp sample and determined the concentration of hydroxyl ions in the liquid phase, which under these conditions amounted to 0.18 g-ion/l Then the slurry from the tank-repulper pump filed in the autoclave (V=0,385 m3) equipped with stirring and heating devices. In the autoclave spent processing the pulp with alkali at T=170oC for 1 hour.

After treatment with alkali slurry of Nickel hydroxide was cooled to 80-90oC and transferred into the supply tank (V=1 m3) before separating the solid and liquid phases. Separating the mother liquor from the precipitate conducted on the filtration centrifuge, where filed cooled to 70-80oC the pulp from the supply tank.

Pressed on the centrifuge sludge with humidity is pout stage wash led purified water at the rate of 2 kg per 1 kg of dry sludge, in the second stage, a solution of 4% barium hydroxide in the amount of 1.5 kg of solution per 1 kg of dry sediment and the third stage is again purified water at the rate of 1.5 kg per 1 kg of dry sediment.

The washed sludge with a moisture content of 15-20% from the centrifuge was transferred to vibrating dryer, where he spent his drying at T=120oC to a moisture content of less than 2%. The dried product was analyzed on the performance of the regulated requirements hydroxide Nickel (II) used for the manufacture of current sources. The results of physico-chemical control of the product obtained had the following characteristics: mass fraction of the sum of Nickel and cobalt - 57,8%, the oxide of Nickel is absent, the mass fraction of barium, related to the mass fraction of the sum of Nickel and cobalt - 2,1%; mass fraction of the sum of the anions Cl-and SO42-(free), related to the mass fraction of Nickel and cobalt - 0,34%, the amorphous phase is missing, the specific volume is 0.65 cm3/g, electrochemical capacitance - 0,166 a/h 1,

Getting hydroxide Ni (II) proposed way faster and cheaper process, as it eliminates lengthy and energy-intensive operation of the sludge drying before washing hydroxide Ni (II) from impurities. In addition, the final product is Holocene hydroxide Nickel (II) current sources, including the preparation of the initial solution of the hydroxide of alkali metal salt of Nickel (II) and barium hydroxide, mixing them, the precipitation of the hydroxide of Nickel (II) separating the mother liquor, washing the precipitate and drying, characterized in that before washing the residue is treated with alkali in an autoclave at a temperature of 130-200oC.

2. The method according to p. 1, characterized in that the alkali treatment is carried out at the concentration of hydroxyl ions in the liquid phase of the pulp, 0.05-0.3 g-ion/liter

3. The method according to p. 1, characterized in that the washing of the precipitate are in three stages: the first stage of water in the second stage with a solution of barium hydroxide with a concentration of 2-6% and in an amount to provide a mass ratio of the solution to precipitate (1-2):1, and in the third stage, again with water.

 

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