CN1036707C - Process for producing cobalt oxalate - Google Patents

Abstract

The present invention discloses a method for producing cobalt oxalate, which mainly comprises the steps of dissolution, impurity removal, synthesis, etc. The method is characterized in that in the dissolution step, a cobalt ingot or cobalt granules are used as raw materials, and sulfuric acid and nitric acid are used as solvents for dissolving cobalt. Cobalt oxalate as a commodity produced by using the method of the present invention is used for processing cobalt powder. Compared with cobalt powder processed by cobalt oxalate as a commodity produced by using the traditional method, the cobalt powder processed by the cobalt oxalate produced by using the method of the present invention has the advantages of small granularity, wide accommodation range, etc.

Description

A kind of cobalt oxalate production method

The present invention relates to a kind of cobalt oxalate production method that is used to process cobalt powder.

At present, the production method of cobalt oxalate has two kinds, and a kind of is cobalt chloride technology, and another kind is a Xiao Suangu technology.Cobalt oxalate as Jinchuan, Gansu company and the production of Ganzhou cobalt smeltery adopts above-mentioned technical process to produce.Though these two kinds of methods can both be produced cobalt oxalate, the raw materials used ore that contains cobalt that is, investment cycle is long.And the cobalt oxalate of producing with this method is reprocessed into cobalt powder, and granularity is big, and the scope of application is placed restrictions on.

The object of the present invention is to provide a kind of cobalt oxalate production method, this method is a raw material with the cobalt ingot, invest little and investment cycle short, the cobalt oxalate of producing with this method is reprocessed into cobalt powder, granularity is little, and is applied widely.

Cobalt oxalate production method of the present invention comprises dissolving, removal of impurities, step such as synthetic.Be characterized in earlier a certain amount of cobalt ingot or cobalt button being placed container, add pure water, sulfuric acid successively, and when heating to 45～70 ℃, add nitric acid again to it.Wherein, the weight proportion of pure water, sulfuric acid and nitric acid is: pure water accounts for 70.77～76.77%, sulfuric acid accounts for 20.56～26.56%, nitric acid accounts for 1.67%～3.67%.After the reaction to 50 minute, pour in another container and cool off, obtain the rose vitriol crystal;

Then, in the rose vitriol crystal, add pure water, and evenly stir, heat to it simultaneously, after 90 ℃, add sodium polysulfide solution and cobalt powder, continue to stir, and make pH value,, remove impurity such as nickel, copper, zinc, lead, arsenic through press filtration less than 4.5;

Then, add hydrochloric acid, make pH value remain on 2.5～3 between, when temperature is reduced to 45 ℃, slowly add clorox again, and continue to heat to 90 ℃, evenly stir after, use the pressure filter press filtration, except that impurity such as de-iron, manganese;

At last, add hydrochloric acid again and stir, to pH value be 0.5 o'clock, add the oxalic acid ammonia solution, and evenly to be stirred to pH value be 1.5, through dewatering, dry, pulverize, mixing and stirring, make cobalt oxalate.

Adopt technique scheme, have the following advantages and effect:

1, be cobalt ingot or cobalt button owing to cobalt oxalate production method of the present invention is raw materials used, need be few with equipment, less investment, and the cycle is short;

2, adopt sulfuric acid and nitric acid to come dissolved cobalt ingot or cobalt button, dissolution rate is fast, the production efficiency height.Cobalt oxalate with method of the present invention is produced is reprocessed into cobalt powder, and its granularity little (less than 0.4 micron) is applied widely.

By the following examples the present invention is described in further detail:

Earlier a certain amount of cobalt ingot (or cobalt button) is put into container, add pure water, sulfuric acid successively, heat after 45～70 ℃, add nitric acid again.The weight proportion of described pure water, sulfuric acid and nitric acid is: pure water accounts for 71.77%, sulfuric acid accounts for 26.5%, nitric acid accounts for 1.73%.React after 50 minutes, pour into and allow its naturally cooling in another container, obtain the rose vitriol crystal.Then, in the rose vitriol crystal, add pure water and evenly stir, heat to it simultaneously, after 90 ℃, sodium polysulfide solution and cobalt powder are slowly evenly added, and continue to stir, to keep pH value less than 4.5, through press filtration repeatedly, remove impurity such as nickel, copper, zinc, lead, arsenic.Then, add hydrochloric acid, make pH value remain on 2.5～3 between, when temperature is reduced to 45 ℃, slowly add clorox again, and continue to heat to 90 ℃, evenly stir after, with pressure filter press filtration repeatedly, remove impurity such as de-iron, manganese, its foreign matter content is met the requirements.At last, add hydrochloric acid again and stir, when pH value is 0.5, add the oxalic acid ammonia solution, and evenly to be stirred to PH be 1.5, make the commodity cobalt oxalate through dewatering, dry, pulverize, mixing and stirring with even thread, first quick and back slow mode.Wherein, pure water, ammoniacal liquor and the oxalic acid of formation oxalic acid ammonia solution account for 76%, 12.8%, 11.2% respectively.The commodity cobalt oxalate made from the described method of present embodiment is reprocessed into cobalt powder, and granularity is little, can reach below 0.4 micron.

Selecting weight proportion for use is 76.7% pure water, 21% sulfuric acid and 2.3% nitric acid, makes the commodity cobalt oxalate according to the described method of the foregoing description, and with the cobalt powder of this cobalt oxalate processing, its granularity is less than 0.4 micron again.

Selecting weight proportion for use is 73.4% pure water, 23% sulfuric acid and 3.6% nitric acid, makes the commodity cobalt oxalate according to the described method of the foregoing description, and with the cobalt powder of this commodity cobalt oxalate processing, its granularity is also less than 0.4 micron again.

Claims (2)

1, a kind of cobalt oxalate production method is characterized in that:

Earlier a certain amount of cobalt ingot or cobalt button are inserted in the container, add pure water, sulfuric acid successively, and heat and make its temperature between 45～70 ℃, add nitric acid again, to quicken its reaction, wherein the weight proportion of pure water, sulfuric acid and nitric acid is respectively 70.77～76.77%, 20.56～26.56% and 1.67～3.67%; After the reaction to 50 minute, pour in another container and cool off, obtain the rose vitriol crystal;

Then, in the rose vitriol crystal, add pure water, and evenly stir, heat to it simultaneously, after 90 ℃, add sodium polysulfide solution and cobalt powder, continue to stir, and make pH value,, remove impurity such as nickel, copper, zinc, lead, arsenic through press filtration less than 4.5;

Then, add hydrochloric acid, make pH value remain on 2.5～3 between, when temperature is reduced to 45 ℃, slowly add clorox again, and continue to heat to 90 ℃, evenly stir after, use the pressure filter press filtration, except that impurity such as de-iron, manganese;

At last, add hydrochloric acid again and stir, to pH value be 0.5 o'clock, add the oxalic acid ammonia solution, and evenly to be stirred to pH value be 1.5, through dewatering, dry, pulverize, mixing and stirring, make cobalt oxalate.

2, production way according to claim 1 is characterized in that the oxalic acid ammonia solution is mixed by pure water, ammoniacal liquor and oxalic acid, and their weight proportion is: pure water 76%, ammoniacal liquor 12.8%, oxalic acid 11.2%.