Method of producing nickel (ii) hydroxide

FIELD: chemistry.

SUBSTANCE: invention can be used in chemical industry. The method of producing nickel (II) hydroxide involves treatment of an acidic solution of nickel (II) sulphate in two steps, at the first step with ammonia water to pH 4-4.5, at the second step with sodium hydroxide to pH 11-12. At the second step, the process is carried out by feeding the suspension from the first step into the sodium hydroxide solution. Further, impurities are washed off from the residue in an ascending stream with variable hydrodynamic conditions. The residue is then pressed and dried.

EFFECT: invention increases purity of the product and uniformity of its grain-size distribution.

3 cl, 3 tbl, 3 ex

 

The invention relates to the field of chemistry, namely to obtain a hydroxide of Nickel (II)primarily used in the electrical industry.

The known method hydroxide Nickel (II) active mass of the positive electrodes of alkaline batteries by infusion of a solution of Nickel sulfate, heated to 80-90°C in an alkaline solution of the same temperature. The resulting suspension of Nickel hydroxide is filtered off, dried and after grinding washed from sodium sulfate and dried. The finished product is additionally boiled in 16%alkali solution for one hour, then washed with water and finally dried. Target product contains 56,2% Nickel, 0.2% sulfate-ion battery and provides a maximum capacity of not less than 1,14 Ah/3G Ni.

The method has the following disadvantages.

1. Phase separation of mother liquor from the precipitate labor-intensive, as the precipitate of Nickel hydroxide has an amorphous structure and has high resistivity when filtering.

2. Three drying requires considerable effort and increases energy consumption.

3. The need for treatment with a solution of alkali finished product lengthens the process and increases the consumption of sodium hydroxide (USSR, ed. testimony 51380 "Way of handling hydrate of oxide of Nickel, IPC C01G 53/04, p, 4; 21B, 25, 1937).

Known also way is of Holocene hydroxide Nickel (II), including the deposition of the pre-prepared initial solutions of sodium hydroxide and Nickel sulfate (II) added as an activator of barium ion. The obtained precipitate was separated by filtration, then dried, washed from sulfate ions, dried again and grind. This method has the following disadvantages.

1. The separation of the mother liquor from the amorphous precipitate of Nickel hydroxide (II)having a high resistivity when filtering, time-consuming, requires a major commitment of time and energy.

2. Double drying and grinding also require more power consumption.

3. The introduction of barium at the stage of synthesis of Nickel hydroxide does not improve the quality of the product, but complicates the process.

(M.A., Dalian, V.V. novoderezhkin and other "Manufacture of electric accumulators", M., "Higher school", 1977, 260-277.)

Another known method includes after deposition of Nickel hydroxide (II), as described above, the separation of the mother liquor, centrifuge sludge, dried to a certain moisture, washing away impurities and a second drying. After first drying the paste is injected with a solution containing ions of cobalt. After the first drying from the party of prefabricated selected laboratory sample and conduct the forecast quality of the product. If the laboratory sample does not meet the t requirements on THE specific volume, get the batch treated with 3%caustic soda solution at a ratio of 1 g of alkali 10-15 g of Nickel hydroxide and lead up to the finished product.

The method has the following disadvantages.

1. High complexity, high costs of time and energy in the separation of mother liquor from the amorphous precipitate of hydroxide Nickel (II).

2. Large inputs of two drying, grinding and classification of the final product.

3. The introduction of barium at the stage of synthesis of Nickel hydroxide and impregnation of sediment after the first drying a solution of cobalt does not lead to the improvement of the quality of the target product, but complicate the process.

4. The activation of Nickel hydroxide additives barium and cobalt prevents the use of the product in other branches of engineering.

5. Introduction operations forecast quality and its correction increases the complexity of the process.

(Patent of the Russian Federation 2138447 "Method of production of Nickel (II) hydroxide", IPC 6 C01G 53/04, publ. 27.09.1999.)

Closest to the claimed invention by the technical essence is a way hydroxide Nickel (II), including the deposition of the interaction of a solution of the hydroxide of an alkali metal salt of Nickel (II)washing the precipitate of impurities, its extraction and drying, characterized in that the deposition of Nickel hydroxide (II) lead to the introduction of Cristallago the rata of Nickel sulfate (II) in a heated 15-30%solution of alkali metal hydroxide, the wash is carried out by treatment of the pulp of the Nickel hydroxide in the column in countercurrent mode when the linear velocity of the upward flow of 5-8 m/h with the imposition of the pulsatile perturbation successively with alkali and water, pressed the precipitate of Nickel hydroxide (II) after drying sift.

However hydroxide Nickel (II) precipitated by sodium hydroxide solution at 65-80°C at T:W=1:(4-7), the precipitate of Nickel hydroxide (II) washed of impurities 3-5%solution of alkali at 45-70°C. Drying of the target product are in the electromagnetic field of the microwave (Patent of the Russian Federation 2208585 "Method of production of Nickel (II) hydroxide", IPC 6 C01G 53/04, publ. 20.07.2003).

As disadvantages of the prototype, we note the need to use as the source of a product of Nickel sulfate of high purity and a wide range of fractional composition of the crystalline Nickel hydroxide (II).

The claimed technical solution solves the problem of expansion of the starting products for the production of hydroxide Nickel (II) and obtain a product of high purity is more uniform particle size distribution.

Defined technical problem is achieved by the fact that the way hydroxide Nickel (II) includes treatment with an alkaline solution, washing the precipitate of impurities in the ascending flow with variable hydrodynamic regime, extraction and drying, characterized in that the working acidic solution of Nickel sulfate(P) are in two stages, at first ammonia water to pH 4-4,5, second sodium hydroxide to pH 11-12. At the second stage of the process is carried out by dosing suspension of the first stage in the solution of sodium hydroxide. In addition, washing hydroxide Nickel (II) lead to an upward flow with a variable hydrodynamic mode when the linear velocity of the upward flow 2-4,8 m/h, and drying is carried out in a convection mode, with the imposition of the electromagnetic field of the microwave frequency at a temperature of 105-115°C.

The essence of the proposed technical solution is that the double sulphate of Nickel and ammonium connection with a lower solubility in aqueous solutions than the Nickel sulfate may be obtained from acidic sulfate solutions, which are waste electroplating plants, caudal uterine solutions medeelektrolitnyj plants and intermediate products recycling alkaline batteries. These solutions in their mode of neutralizing ammonia water crystallize in the pH range of 3-4 .5. Following neutralization of the solution results in the precipitation of hydroxides Primastic elements that are not part of the structure of double salts and can be removed from the reaction zone by simple decanting the mother liquor, or in the process of fractionation in an upward flow. While the resulting Nickel hydroxide, p. the essence, repeats the grading of the double salt with a predominant content of the fractions in the range of 20-30 microns. The essence of the proposed technical solution is confirmed by the examples.

Example 1. Starting materials for the synthesis of Nickel hydroxide: model Nickel sulfate solutions containing 150 g/l with NISO4and pH=1,5, ammonia water of 25%sodium hydroxide. Fill the reactor Nickel sulfate solution and with constant stirring, pour the ammonia water to pH of 4.3. Received double salt is filtered off and washed with pulsation in the column in countercurrent mode when the linear velocity of the upward flow of 6 m/h In the reactor with a stirrer to prepare an alkaline solution with a pH of 11-12 and sprinkled double salt to the ratio of T:W=1:6. The resulting suspension is sent for washing in the top part of the pulse columns. Washing hydroxide Nickel lead in counter-current with water linear velocity of the upward flow of 1-6 m/H. Shipping laundered spherical Nickel hydroxide passes through the lower part of the columns. Washed spherical Nickel hydroxide with T:W=1:3 squeezed and dried in convective mode with the imposition of the electromagnetic field of the microwave frequency at a temperature of 105-115°C. the Spent wash water are removed through the overflow pipe in the upper part of the column and is collected in the sump. Fine frequent the sludge, represents a hydroxide of Nickel, not corresponding to THE granulometric composition in an amount of 4-12%, captured in the sump. Process indicators hydroxide of Nickel are shown in table 1.

Table 1
Selection of the mode of washing hydroxide Nickel
The speed of the upward flow, m/hThe result of washing
1Does not meet the requirements of TU. The high content of fine fraction and sulfate ions in the product.
2Meets the requirements of TU. Direct yield of 98%. Boundary content of the fine fraction and sulfate ions in the product. Small equipment performance.
3Meets the requirements of TU. Direct yield of 97%.
4Meets the requirements of TU. Direct yield of 96.5%.
5Meets the requirements of TU. Direct yield of 94%.
6Meets the requirements is to be THAT. Direct yield of 90%. Increased entrainment product.

Example 2. Starting materials for the synthesis of Nickel hydroxide: sulfuric acid Nickel solution, ammonia water 25% sodium hydroxide. Fill the reactor Nickel sulfate solution and with constant stirring dosed ammonia water to pH 2-5. The resulting slurry incubated 15 minutes with constant stirring. The double salt is separated from the solution by decantation. The process of deposition of Nickel hydroxide are similar to example 1. Washing the suspension is carried out analogously to example 1 at a linear velocity of the upward flow of 4 m/h process Indicators hydroxide Nickel are presented in table 2.

Table 2
The selection of the processing mode of the ammonia water
Neutralization of sulfuric acid Nickel solution to pHResult
2,0Meets the requirements of TU. Direct yield of 44%.
2,5Meets the requirements of TU. Direct yield of 67%.
3,0Meets the requirements of TU. Direct o is d product of 88%.
3,5Meets the requirements of TU. Direct yield of 92%.
4,0Meets the requirements of TU. Direct yield of 95%.
4,5Meets the requirements of TU. Direct yield of 96%.
5,0Meets the requirements of TU. Direct yield of 96%.

Example 3. Starting materials for the synthesis of Nickel hydroxide: sulfuric acid Nickel solution, ammonia water 25% sodium hydroxide. Fill the reactor Nickel sulfate solution and with constant stirring dosed ammonia water to pH 4.5. The resulting slurry incubated 15 minutes with constant stirring. In the resulting slurry double salt pour in a solution of sodium hydroxide to a pH of 5-9. Washing the suspension is carried out analogously to example 1 at a linear velocity of the upward flow of 4 m/h process Indicators hydroxide Nickel are presented in table 3.

Table 3
Selection of processing mode lye
Processing pulp double salts with sodium hydroxide solution on the pH Result
5,0Does not meet the requirements of TU. The high content of sulfate ions.
5,5Does not meet the requirements of TU. The high content of sulfate ions.
6,0Meets the requirements of TU. Direct yield 92%
6,5Meets the requirements of TU. Direct yield of 94%.
7,0Meets the requirements of TU. Direct yield of 96%.
7,5Meets the requirements of TU. Direct yield of 96%. Increased consumption of alkali.
8,0Meets the requirements of TU. Direct yield of 96%. Increased consumption of alkali.
9,0Meets the requirements of TU. Direct yield of 96%. Increased consumption of alkali.

1. The way hydroxide Nickel (II)includes treatment with an alkaline solution, washing the precipitate of impurities in the ascending flow with variable hydrodynamic regime, extraction and drying, characterized in that education is otcu acidic solution of Nickel sulfate (II) are in two stages, at first ammonia water to pH 4-4,5, second sodium hydroxide to pH 11-12.

2. The method according to claim 1, characterized in that in the second stage process is carried out by dosing suspension of the first stage in the sodium hydroxide solution.

3. The method according to claim 1, characterized in that the washing hydroxide Nickel (II) lead to an upward flow with a variable hydrodynamic mode when the linear velocity of the upward flow 2-4,8 m/h, and drying is carried out in a convection mode, with the imposition of the electromagnetic field of the microwave frequency at a temperature of 105-115°C.



 

Same patents:

FIELD: power engineering.

SUBSTANCE: method to produce a composite NiO/C material containing 15-60% NiO and representing crystallites β-NiO evenly distributed on a carbon carrier surface with the average size of 2-5 nm, is based on production of NiO nanoparticles as a result of electrochemical oxidation and destruction of two nickel electrodes in solutions of alkaline metal hydroxides with concentration of 2 mole/l under action of AC current with frequency of 50 Hz at average value of current referred to a unit of electrode surface area making 0.3-1.5 A/cm2, with simultaneous deposition of produced nickel oxide nanoparticles onto the carbon carrier, subsequent filtration of the produced suspension, washing of composite by distilled water and its drying at 80°C for 1 hour.

EFFECT: invention makes it possible to increase quality of produced material due to absence of admixtures and to reduce costs for its production.

4 ex

FIELD: process engineering.

SUBSTANCE: invention relates to device and method of producing compounds by precipitation of solid substances. Proposed device comprises reactor provided with inclined settler. Proposed method comprises mixing initial substances in reactor, precipitation of compounds in reaction zone, partial separation of mother leach from precipitated product in inclined settler, separation of product suspension, its filtration and drying. Invention covers also mixed powder of nickel-cobalt hydroxide with WET-surface of less than 20 m2/g and impact density exceeding 2.4 g/cm3.

EFFECT: suspension with concentration exceeding stoichiometric one.

29 cl, 13 dwg, 5 ex

The invention relates to the field of non-ferrous metallurgy and can be used in the battery industry

The invention relates to the field of technology of inorganic and electrochemical industries, specifically to methods of producing powders for filling the electrode cells of the Nickel batteries electrochemical elements, as well as to the production technology of catalysts

The invention relates to chemistry and can be used in the electrical industry, as well as in the production of enamels, glass, and for synthesis of other compounds Nickel

The invention relates to the field of chemical technology, particularly to a material based on Nickel hydroxide used in electrochemical elements

The invention relates to electrochemistry, in particular, compositions of hydrate of oxide of Nickel used in the production of chemical current sources

The invention relates to the production of nanostructured materials by chemical means
The invention relates to ferrous metallurgy and can be used to produce spherical hydrate of oxide of Nickel used in the battery industry
The invention relates to the field of production of Nickel compounds, hydroxides, and can be used in the manufacture of alkaline batteries

FIELD: process engineering.

SUBSTANCE: invention relates to device and method of producing compounds by precipitation of solid substances. Proposed device comprises reactor provided with inclined settler. Proposed method comprises mixing initial substances in reactor, precipitation of compounds in reaction zone, partial separation of mother leach from precipitated product in inclined settler, separation of product suspension, its filtration and drying. Invention covers also mixed powder of nickel-cobalt hydroxide with WET-surface of less than 20 m2/g and impact density exceeding 2.4 g/cm3.

EFFECT: suspension with concentration exceeding stoichiometric one.

29 cl, 13 dwg, 5 ex

FIELD: power engineering.

SUBSTANCE: method to produce a composite NiO/C material containing 15-60% NiO and representing crystallites β-NiO evenly distributed on a carbon carrier surface with the average size of 2-5 nm, is based on production of NiO nanoparticles as a result of electrochemical oxidation and destruction of two nickel electrodes in solutions of alkaline metal hydroxides with concentration of 2 mole/l under action of AC current with frequency of 50 Hz at average value of current referred to a unit of electrode surface area making 0.3-1.5 A/cm2, with simultaneous deposition of produced nickel oxide nanoparticles onto the carbon carrier, subsequent filtration of the produced suspension, washing of composite by distilled water and its drying at 80°C for 1 hour.

EFFECT: invention makes it possible to increase quality of produced material due to absence of admixtures and to reduce costs for its production.

4 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in chemical industry. The method of producing nickel (II) hydroxide involves treatment of an acidic solution of nickel (II) sulphate in two steps, at the first step with ammonia water to pH 4-4.5, at the second step with sodium hydroxide to pH 11-12. At the second step, the process is carried out by feeding the suspension from the first step into the sodium hydroxide solution. Further, impurities are washed off from the residue in an ascending stream with variable hydrodynamic conditions. The residue is then pressed and dried.

EFFECT: invention increases purity of the product and uniformity of its grain-size distribution.

3 cl, 3 tbl, 3 ex

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

FIELD: metallurgy.

SUBSTANCE: method comprises production of the nickel oxide powder from metal nickel electrodes by electrolysis in basic solution of sodium hydroxide. Process is executed at temperature 20-30°C upon simultaneous action on the electrodes of current with frequency 20 Hz. At that electrolysis is performed at asymmetrical alternating current with current density of anode and cathode half cycle 2.5 A/cm2 and 1 A/cm2, respectively, and at action on the electrodes of the ultrasound radiation with frequency from 150 to 300 kHz.

EFFECT: production of ultra-micro-dispersed powder of nickel oxide suitable for use during catalitic production of nano-carbon materials with maximum production of the target product, decreasing of power consumption.

6 ex

FIELD: electrical engineering.

SUBSTANCE: invention relates to electrical engineering, namely to production of aqueous paste of nickelous hydroxide. As starting material used is alkaline industrial effluents directly from section of producing metal ceramic nickel oxide electrodes containing admixture KOH, K2SO4 and hydrate suspension, which are settled, then suspension is washed and filtered.

EFFECT: invention enables to obtain fine highly active fraction of nickelous hydroxide with simplification of method.

4 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to electrochemical production of active forms of nanoparticles of metal oxides. Electrochemical method of producing nano-sized structures of nickel (II) oxide involves oxidation of anode in ionic liquid in an air atmosphere. Nickel anode and cathode are used. Oxidation is performed at temperature 20-25 °C for 2-20 minutes, with density of direct current of 5-10 mA/cm2 or at constant potential of 2.3-5 V. Ionic liquid is preferably with addition of distilled water or propylene glycol.

EFFECT: invention ensures production of highly ordered nano-sized structures.

4 cl, 5 dwg, 5 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to a method of producing crystalline nanopowders of metals with the size of crystallites of less than ≤ 10 nm and can be used in chemical industry, for production of intermediate products for fine ceramic materials. Synthesis is carried out in a water-organic medium using as sources of metal nitrates, chlorides or acetates. For formation and stabilization of sol used are acetylacetone-alcoholic solutions of N,N-dimethyloctylamine, hexamethylene tetramine or monoethanolamine. As a complexing agent used is acetylacetone. Obtained sol through a jet nozzle is dispersed into liquid nitrogen, where at the cooling rate > 30° cryogranulating takes place. Produced granules are subjected to vacuum-sublimation drying to form a cryo-airgel, which is then annealed at 500 °C in air for 3 hours.

EFFECT: proposed method provides technologically effective and environmentally acceptable method of producing nanocrystalline of metal oxides.

4 cl, 8 dwg, 1 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: method of producing nanodispersed metal oxides involves forming a reaction mixture by introducing metal and carbamide nitrates into the aqueous medium in a stoichiometric ratio. The reaction medium is exposed to microwave radiation. The reaction mixture is formed directly in the reaction volume at the following component ratio, wt %: a mixture of nitrate and carbamide 10-20, water - the rest. The exposure to microwave radiation is carried out with open access to the reaction medium in the reaction volume. The intermediate reaction product is dried at a temperature of, at least, 200°C. The dried product is ground to a particle size of not more than 20 nm. During the grinding of the dried product, a hydrophobizing treatment is carried out in parallel with a hydrophobizing mixture consisting of silanes and silicone oligomers taken in the ratio, wt %: silane 17-33, silicone oligomer 67-83.

EFFECT: complete conversion of metal nitrates to oxides having prolonged resistance to agglomeration, increasing the yield of products, excluding the presence of traces of the original components in the products.

4 cl, 6 tbl, 8 ex

Up!