Summary of the invention
The object of the present invention is to provide a kind of preparation method of with low cost, non-crystalline state nickelous sulfide that production efficiency is high.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for non-crystalline state nickelous sulfide, concrete steps are as follows:
A, sodium sulphite dissolve
The tap water that is 5 ~ 25 ℃ by temperature joins in sodium sulphite dissolving tank, add stablizer, stablizer and tap water volume ratio are 0.18 ~ 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve postcure na concn and be controlled at 90 ~ 120g/l, stir 1 ~ 1.5 hour, add dispersion agent, dispersion agent and tap water volume ratio are 0.15 ~ 0.2:100 again, stir 0.5 ~ 1 hour;
B, the preparation of non-crystalline state nickelous sulfide
Another extracting container adds liquid after copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 ℃, pH value is 3.2 ~ 3.6, adds sodium sulphite anhydrous 99.3, stirs 0.5 ~ 1 hour, after S-WAT dissolves, concentration is 0.8 ~ 1g/l, add dispersion agent, after dispersion agent and copper, liquid volume ratio is 0.2 ~ 0.25:100 again, stirs 15 ~ 30 minutes; By the sodium sulfide solution of step a and above-mentioned solution by volume 1.0 ~ 1.3:1 mix, stir and within 0.5 ~ 1 hour, make non-crystalline state nickelous sulfide pulp liquid.
In described step b, add dispersion agent and stablizer, can keep for a long time it to remove copper activity.
Described dispersion agent is that polyoxyethylene glycol, the stablizer of purity 99% is the hydrazine hydrate of massfraction 80%.
The present invention has significantly different from traditional nickelous sulfide preparation method: sodium sulphite has added stablizer while dissolving, prevents the oxidation of sodium sulphite, guarantees to add dispersion agent by system reducing simultaneously, prevents from forming between sodium sulphite polysulfide.After copper, liquid adds reductive agent, makes system prepared by nickelous sulfide present reductibility.When preparation, control add-on the uniform stirring of sodium sulphite, prevent that local sulphur source is excessive, form polysulfide, add dispersion agent simultaneously, reduce the probability of collision between nickelous sulfide, can keep for a long time active.Nickelous sulfide prepared by traditional method was placed after 24 hours in air, except copper activity reduces gradually, placed and exceeded after 48 hours, and activity is down to 15% ~ 20%.Non-crystalline state nickelous sulfide of the present invention is placed 7 days in air, except copper activity still can keep 80% ~ 90%.
Embodiment
A preparation method for non-crystalline state nickelous sulfide, concrete steps are as follows:
A, sodium sulphite dissolve
The tap water that is 5 ~ 25 ℃ by temperature joins in sodium sulphite dissolving tank, add stablizer, stablizer and tap water volume ratio are 0.18 ~ 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve postcure na concn and be controlled at 90 ~ 120g/l, stir 1 ~ 1.5 hour, add dispersion agent, dispersion agent and tap water volume ratio are 0.15 ~ 0.2:100 again, stir 0.5 ~ 1 hour;
B, the preparation of non-crystalline state nickelous sulfide
Another extracting container adds liquid after copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 ℃, pH value is 3.2 ~ 3.6, adds sodium sulphite anhydrous 99.3, stirs 0.5 ~ 1 hour, after S-WAT dissolves, concentration is 0.8 ~ 1g/l, add dispersion agent, after dispersion agent and copper, liquid volume ratio is 0.2 ~ 0.25:100 again, stirs 15 ~ 30 minutes; By the sodium sulfide solution of step a and above-mentioned solution by volume 1.0 ~ 1.3:1 mix, stir and within 0.5 ~ 1 hour, make non-crystalline state nickelous sulfide pulp liquid.
In described step b, add dispersion agent and stablizer, can keep for a long time it to remove copper activity.
Described dispersion agent is that polyoxyethylene glycol, the stablizer of purity 99% is the hydrazine hydrate of massfraction 80%.
Embodiment 1
A preparation method for non-crystalline state nickelous sulfide, concrete steps are as follows:
A, sodium sulphite dissolve
The tap water that is 5 ~ 25 ℃ by temperature joins in sodium sulphite dissolving tank, add stablizer, stablizer and tap water volume ratio are 0.18:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve postcure na concn and be controlled at 90g/l, stir 1 ~ 1.5 hour, add dispersion agent, dispersion agent and tap water volume ratio are 0.15:100 again, stir 0.5 ~ 1 hour;
B, the preparation of non-crystalline state nickelous sulfide
Another extracting container adds liquid after copper removal, nickel concentration 75g/l in liquid after copper removal, temperature is 20 ~ 40 ℃, pH value is 3.2 ~ 3.6, adds sodium sulphite anhydrous 99.3, stirs 0.5 ~ 1 hour, after S-WAT dissolves, concentration is 0.8g/l, add dispersion agent, after dispersion agent and copper, liquid volume ratio is 0.2:100 again, stirs 15 ~ 30 minutes; By the sodium sulfide solution of step a and above-mentioned solution by volume 1.0:1 mix, stir and within 0.5 ~ 1 hour, make non-crystalline state nickelous sulfide pulp liquid.
Embodiment 2
A preparation method for non-crystalline state nickelous sulfide, concrete steps are as follows:
A, sodium sulphite dissolve
The tap water that is 5 ~ 25 ℃ by temperature joins in sodium sulphite dissolving tank, add stablizer, stablizer and tap water volume ratio are 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve postcure na concn and be controlled at 120g/l, stir 1 ~ 1.5 hour, add dispersion agent, dispersion agent and tap water volume ratio are 0.2:100 again, stir 0.5 ~ 1 hour;
B, the preparation of non-crystalline state nickelous sulfide
Another extracting container adds liquid after copper removal, nickel concentration 85g/l in liquid after copper removal, temperature is 20 ~ 40 ℃, pH value is 3.2 ~ 3.6, adds sodium sulphite anhydrous 99.3, stirs 0.5 ~ 1 hour, after S-WAT dissolves, concentration is 1g/l, add dispersion agent, after dispersion agent and copper, liquid volume ratio is 0.25:100 again, stirs 15 ~ 30 minutes; By the sodium sulfide solution of step a and above-mentioned solution by volume 1.3:1 mix, stir and within 0.5 ~ 1 hour, make non-crystalline state nickelous sulfide pulp liquid.
Embodiment 3
A preparation method for non-crystalline state nickelous sulfide, concrete steps are as follows:
A, sodium sulphite dissolve
The tap water that is 5 ~ 25 ℃ by temperature joins in sodium sulphite dissolving tank, add stablizer, stablizer and tap water volume ratio are 0.2:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve postcure na concn and be controlled at 100g/l, stir 1 ~ 1.5 hour, add dispersion agent, dispersion agent and tap water volume ratio are 0.16:100 again, stir 0.5 ~ 1 hour;
B, the preparation of non-crystalline state nickelous sulfide
Another extracting container adds liquid after copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 ℃, pH value is 3.2 ~ 3.6, adds sodium sulphite anhydrous 99.3, stirs 0.5 ~ 1 hour, after S-WAT dissolves, concentration is 0.9g/l, add dispersion agent, after dispersion agent and copper, liquid volume ratio is 0.21:100 again, stirs 15 ~ 30 minutes; By the sodium sulfide solution of step a and above-mentioned solution by volume 1.1:1 mix, stir and within 0.5 ~ 1 hour, make non-crystalline state nickelous sulfide pulp liquid.
Non-crystalline state nickelous sulfide prepared by embodiment 1 is placed the non-crystalline state nickelous sulfide of 7 days, embodiment 2 preparing and is placed the non-crystalline state nickelous sulfide of 14 days, embodiment 3 preparing and place 20 days, carry out copper-stripping reaction and check that it removes copper activity, non-crystalline state nickelous sulfide add-on be after iron liquid 0.7%, after copper removal, liquid is containing copper number all in 0.8 ~ 2.5ppm value range, and non-crystalline state nickelous sulfide copper removal activity keeping is better.
Non-crystalline state nickelous sulfide temporal evolution copper removal active testing data sheet 1.As can be seen from Table 1, non-crystalline state nickelous sulfide, placing respectively after 7 days, 14 days and 20 days, carries out copper removal test, and after copper removal, the requirement of hydroful foot nickel electrowinning, illustrates that non-crystalline state nickelous sulfide copper removal activity keeping is better.
In table, refer to " storage period " the aerial storage period of non-crystalline state nickelous sulfide of preparation, " liquid cupric before copper removal " is to place 7 days at non-crystalline state nickelous sulfide, liquid copper content after the iron got at the scene when 14 days and 20 days, " nickelous sulfide and copper additional proportion " refer to liquid after non-crystalline state nickelous sulfide adds volume to be iron in test non-crystalline state nickelous sulfide activity test process long-pending 0.7%, " liquid cupric after copper removal " refers to non-crystalline state nickelous sulfide placement 7 days, after 14 days and 20 days, " copper removal before liquid " carried out to liquid copper content after copper removal that copper removal obtains, " cupric ion decreasing ratio " refers to that the cupric ion of removing accounts for the total amount of total ion.