CN103864157A - Preparation method of amorphous nickel sulfide - Google Patents

Preparation method of amorphous nickel sulfide Download PDF

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CN103864157A
CN103864157A CN201410074075.4A CN201410074075A CN103864157A CN 103864157 A CN103864157 A CN 103864157A CN 201410074075 A CN201410074075 A CN 201410074075A CN 103864157 A CN103864157 A CN 103864157A
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sulfide
copper
dispersion agent
nickel sulfide
preparation
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CN103864157B (en
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郭勇
陈自江
郑军福
赵重
卢建波
王得祥
刘冬莉
朱纪念
翟惠明
王立成
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Jinchuan Group Nickel Cobalt Co ltd
Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
Jinchuan Group Co Ltd
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Abstract

The invention relates to a chemical purification method, and in particular relates to a preparation method of amorphous nickel sulfide. The preparation method provided by the invention is obviously different from the traditional nickel sulfide preparation method and is characterized in that a stabilizer is added when sodium sulfide is dissolved, so that the oxidation of the sodium sulfide is avoided and the system reducibility is ensured at the same time; a dispersant is added, so that a polysulfide is prevented from formed in the sodium sulfide; and a reducing agent is added into a copper suspension, so that the reducibility of the system for preparing the nickel sulfide is presented. When the amorphous nickel sulfide is prepared, the adding quantity of the sodium sulfide is controlled and the even stirring is carried out, so that the local excess sulfur source is avoided, namely, the polysulfide formed due to the local excess sulfur source is avoided; and meanwhile, the dispersant is added, so that the collision probability among the nickel sulfides is reduced, namely, the activity of nickel sulfide is maintained for a long time. According to the traditional method, after the prepared nickel sulfide is placed in the air for 24 hours, the copper removal activity of the nickel sulfide is gradually decreased; and after the prepared nickel sulfide is placed in the air for 48 hours, the copper removal activity of the nickel sulfide is decreased to 15% to 20%. According to the method provided by the invention, after the amorphous nickel sulfide is placed in the air for 7 days, the copper removal activity of the amorphous nickel sulfide can be still maintained at 80% to 90%.

Description

A kind of preparation method of non-crystalline state nickelous sulfide
Technical field
The present invention relates to chemical industry purifying method, particularly a kind of preparation method of non-crystalline state nickelous sulfide.
Background technology
In traditional nickelous sulfide preparation process, directly sodium sulphite is dissolved, then join after copper reaction in liquid and generate nickelous sulfide.In the time that sodium sulphite dissolves, owing to containing a small amount of dissolved oxygen in solution, can react after running into the sodium sulphite of reductibility, oxidized portion sodium sulphite, the consumption of sodium sulphite rises, and utilization ratio declines; Sodium sulphite joins after copper removal and in liquid, reacts and generate nickel sulphide solids particle, because grain graininess is little, surface atom ratio is large, specific surface area is large, surface can be large, and in energy unsteady state, nickel sulphide solids particle all trends towards flocking together, the reunion of nickelous sulfide occurs, and production efficiency is low.
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%.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
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.
Figure 2014100740754100002DEST_PATH_IMAGE002
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.

Claims (3)

1. a preparation method for non-crystalline state nickelous sulfide, is characterized in that 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.
2. require described a kind of copper-removing method according to right 1, it is characterized in that adding dispersion agent and stablizer in described step b, can keep for a long time it to remove copper activity.
3. require described a kind of copper-removing method according to right 1, it is characterized in that described dispersion agent is that polyoxyethylene glycol, the stablizer of purity 99% is the hydrazine hydrate of massfraction 80%.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110156093A (en) * 2019-05-30 2019-08-23 重庆交通大学 The method of nickel sulfide ultra-fine grain is efficiently prepared under a kind of temperate condition
CN113151863A (en) * 2021-03-18 2021-07-23 金川集团股份有限公司 Method for removing copper ions in nickel production process by electrodeposition

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CN101186346A (en) * 2007-12-19 2008-05-28 扬州大学 Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110156093A (en) * 2019-05-30 2019-08-23 重庆交通大学 The method of nickel sulfide ultra-fine grain is efficiently prepared under a kind of temperate condition
CN110156093B (en) * 2019-05-30 2022-03-11 重庆交通大学 Method for efficiently preparing nickel sulfide ultrafine particles under mild condition
CN113151863A (en) * 2021-03-18 2021-07-23 金川集团股份有限公司 Method for removing copper ions in nickel production process by electrodeposition

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