CN106191917A - A kind of impurity removal process of nickle electrolysis anode solution - Google Patents

Abstract

A process for removing impurities in a nickel electrolysis anolyte, the method comprising the following steps: (1) the nickel electrolysis anolyte contains ammonium chloride in a concentration range of 30 to 300 g/L, a nickel ion concentration in a range of 0.5 to 100 g/L, copper The ion concentration range is 0.5-10g/L, and the iron ion concentration range is 0.01-2g/L. Take nickel electrolysis anolyte, add nickel sulfide to make the concentration range 0.5-20g/L, control the temperature at 20-70°C, and magnetically stir Rotate at 300-700r/min, stir for 10-120min, filter, and the filtrate is the nickel electrolysis anolyte after copper removal; (2) Add ammonia water to the nickel electrolysis anolyte after copper removal to make the concentration 30-400g/L , stirred for 1 to 20 minutes, and filtered to obtain the nickel electrolysis anolyte after iron removal. The process has the advantages of simple process, simple and easy-to-obtain raw materials, no introduction of other impurities in the process, and excellent copper and iron removal effect.

Description

A kind of impurity removal process for nickel electrolytic anolyte

(1) Technical field

The invention relates to a process for removing impurities of nickel electrolytic anolyte, which belongs to the technical field of hydrometallurgy.

(2) Background technology

In the current industrial production of electrolytic nickel, the sulfuric acid system is mainly used to electrolyze nickel. After decades of transformation and innovation, this process has been continuously improved and has become increasingly mature. However, with the development of society and the advancement of technology, the traditional nickel electroplating The shortcomings of the technology are increasingly revealed in the production. The disadvantages of the traditional electrolytic nickel process are as follows:

1. Using the acid system electrodeposition nickel process, using boric acid as a buffer, it is necessary to strictly control the pH within the range of 4.5 to 5.4. If the pH is too low, the efficiency of the cathode will decrease, and if the pH is too high, it will lead to the formation of nickel hydroxide. Nickel The physical properties and morphology deteriorate.

2. In the acidic system, the content and types of impurities in the anolyte during the electrolysis process are many, and the impurity removal process in the acidic system is complicated and the process cost is high.

Therefore, the electrolytic nickel method of the ammonium complex system, which is relatively efficient and green, and the technological process is relatively simple, can be applied to mechanized automatic production, increase production capacity, and expand the pH range of the buffer additive has great significance for the industrial production of electroplated nickel, and it is self-evident. It is also in line with the current green production policy advocated by the country, and the electrolysis of the ammonium chloride system as the anolyte can be configured into an ammonia complex system electrolyte that meets the requirements of cathodic electrodeposition. Copper and iron are the main impurities in the anolyte, but in There is almost no research on the method of removing copper and iron in the ammonium chloride system.

The invention proposes a method for removing copper and iron in an ammonium chloride system, which has huge prospects, environmental and economic benefits when used in the electrolysis of nickel in an ammonium complex alkaline system.

(3) Contents of the invention

The purpose of the present invention is to propose a nickel matte leaching and impurity removal process in alkaline electrolyte for the almost non-existent problem of ammonia complex alkaline system electrolysis of nickel to remove copper and iron, by electrolyzing nickel anolyte in ammonium chloride system In the process, adding nickel sulfide to remove copper and adding ammonia water to remove iron can effectively remove impurities and successfully obtain an electrolyte with copper and iron content up to the standard. Iron effect is excellent and so on.

To achieve the above object, the present invention adopts the following technical solutions:

A kind of impurity removal process of nickel electrolysis anolyte, described method comprises the following steps:

(1) Nickel electrolysis anolyte contains ammonium chloride concentration range of 30-300g/L, nickel ion concentration range of 0.5-100g/L, copper ion concentration range of 0.5-10g/L, iron ion concentration range of 0.01-2g /L, take nickel electrolysis anolyte, add nickel sulfide to make the concentration range 0.5~20g/L, control temperature 20~70℃, magnetic stirring speed 300~700r/min, stir for 10~120min, filter, the filtrate is Nickel electrolytic anolyte after copper removal;

(2) Add ammonia water to the nickel electrolytic anolyte after copper removal to make the concentration 30-400g/L, stir for 1-20min, and filter to obtain the nickel electrolytic anolyte after iron removal, which is used for cathodic electrodeposition to prepare nickel.

Further, in step (1), the concentration of the ammonium chloride is preferably 50-200 g/L.

Further, in step (1), the nickel ion concentration is preferably 5-80 g/L.

Further, in step (1), the copper ion concentration is preferably 1-5 g/L.

Further, in step (1), the iron ion concentration is preferably 0.05-1 g/L.

Furthermore, in step (1), the nickel sulfide concentration is preferably 1-10 g.

Further, in step (1), the temperature range is preferably 40-60°C.

Further, in step (1), the magnetic stirring speed is preferably 400-600 r/min.

Further, in step (1), the stirring time is preferably 20-80 min.

Further, in step (2), the concentration of ammonia water is preferably 50-250 g/L.

Further, in step (2), the stirring time is preferably 3-10 min.

Further, the preparation consists of steps (1) to (2).

The anode corresponding to the nickel electrolysis anolyte in the present invention is high matte nickel.

The beneficial effects of the invention are: the invention solves the problem of removing impurity copper and iron from the anolyte in the nickel-ammonia alkaline electrolysis system, and the effect can meet the industrial demand. The raw materials required by the invention can be recycled, the technological process is simple, green and environment-friendly, and has huge prospects, environment and economic benefits.

(4) Description of drawings

Fig. 1 is the scanning electron micrograph of embodiment 3 electroplating nickel.

(5) Specific implementation methods

The present invention will be further described below through specific examples, but the protection scope of the present invention is not limited thereto.

Example 1

Get containing ammonium chloride concentration 30g/L, nickel ion concentration is 0.5g/L, copper ion concentration is 0.5g/L, iron ion concentration is 0.01g/L, gets electrolyte 1L in the beaker, adds nickel sulfide, its The mass is 0.5g, the temperature is controlled at 20°C, and the magnetic stirring speed is 700r/min. After stirring for 10 minutes, filter, and the filtrate is the electrolyte after copper removal. Add ammonia water to the electrolytic solution after copper removal to make the concentration 30g/L, stir with a glass rod for 1min, and filter to obtain an electrolytic solution after iron removal, which is used for cathodic electrodeposition to prepare nickel.

Based on Example 1, the copper removal rate was 99.21%, and the iron removal rate was 98.57%.

The nickel-plated layer obtained in Example 1 was macroscopically observed and characterized by SEM. The macroscopic appearance of the nickel-plated layer was bright and smooth, and the microscopic appearance was smooth and compact.

Example 2

Take the ammonium chloride concentration of 300g/L, nickel ion concentration of 100g/L, copper ion concentration of 10g/L, iron ion concentration of 2g/L, take 1L of electrolyte solution in a beaker, add nickel sulfide, its mass is 20g , control the temperature at 70°C, and the magnetic stirring speed is 300r/min. After stirring for 120min, filter, and the filtrate is the electrolyte solution after copper removal. Then add 400g/L ammonia water to the electrolytic solution after copper removal, stir with a glass rod for 20 minutes, and filter to obtain an electrolytic solution after iron removal, which is used for cathodic electrodeposition to prepare nickel.

Based on Example 2, the copper removal rate was 98.88%, and the iron removal rate was 97.27%.

The nickel-plated layer obtained in Example 1 was macroscopically observed and characterized by SEM. The macroscopic appearance of the nickel-plated layer was bright and smooth, and the microscopic appearance was smooth and compact.

Example 3

Take 50g/L of ammonium chloride concentration, 5g/L of nickel ion concentration, 1g/L of copper ion concentration, and 0.05g/L of iron ion concentration, take 1L of electrolyte solution in a beaker, add nickel sulfide, and its mass is 1g, controlled temperature 40°C, magnetic stirring speed 400r/min, stirred for 80min, filtered, and the filtrate was the electrolytic solution after copper removal. Add 50 g/L ammonia water to the electrolytic solution after copper removal, stir with a glass rod for 3 minutes, and filter to obtain an electrolytic solution after deironing, which is used for cathodic electrodeposition to prepare nickel.

The copper removal rate based on Example 3 was 99.57%, and the iron removal rate was 98.65%.

The nickel-plated layer obtained in Example 3 was macroscopically observed and characterized by SEM. The macroscopic appearance of the nickel-plated layer was bright and smooth, and the microscopic appearance was smooth and compact.

Example 4

Take 200g/L of ammonium chloride concentration, 80g/L of nickel ion concentration, 5g/L of copper ion concentration, and 1g/L of iron ion concentration, take 1L of electrolyte solution in a beaker, add nickel sulfide, and its mass is 10g , control the temperature at 60° C., and the magnetic stirring speed at 600 r/min. After stirring for 20 minutes, filter, and the filtrate is the electrolyte after copper removal. Add 250 g/L ammonia water to the electrolytic solution after copper removal, stir with a glass rod for 10 minutes, and filter to obtain an electrolytic solution after deironing, which is used for cathodic electrodeposition to prepare nickel.

The copper removal rate based on Example 4 was 98.79%, and the iron removal rate was 99.11%.

The nickel-plated layer obtained in Example 4 was macroscopically observed and characterized by SEM. The macroscopic appearance of the nickel-plated layer was bright and smooth, and the microscopic appearance was smooth and compact.

Example 5

Take 125g/L of ammonium chloride concentration, 40g/L of nickel ion concentration, 2.5g/L of copper ion concentration, and 0.5g/L of iron ion concentration, take 1L of electrolyte in a beaker, add nickel sulfide, its mass 5g, controlled temperature 50°C, magnetic stirring speed 500r/min, stirred for 40min, filtered, and the filtrate was the electrolytic solution after copper removal. Add 120 g/L ammonia water to the electrolytic solution after copper removal, stir with a glass rod for 5 minutes, and filter to obtain an electrolytic solution after deironing, which is used for cathodic electrodeposition to prepare nickel.

The copper removal rate based on Example 5 was 99.53%, and the iron removal rate was 99.32%.

The nickel-plated layer obtained in Example 5 was macroscopically observed and characterized by SEM. The macroscopic appearance of the nickel-plated layer was bright and smooth, and the microscopic appearance was smooth and compact.

Claims (6)

1. an impurity removal process for nickle electrolysis anode solution, said method comprising the steps of:

(1) nickle electrolysis anode solution containing ammonium chloride concentration range be 30～300g/L, nickel ion concentration scope be 0.5～100g/L, Copper ion concentration scope is 0.5～10g/L, iron concentration scope is 0.01～2g/L, takes nickle electrolysis anode solution, adds sulfuration Nickel makes its concentration range be 0.5～20g/L, control temperature 20～70 DEG C, and magnetic agitation rotating speed 300～700r/min stirs 10 ～after 120min, filter, filtrate is the nickle electrolysis anode solution after copper removal；

(2) the nickle electrolysis anode solution addition ammonia after copper removal makes its concentration be 30～400g/L, stirs 1～20min, filters After, the nickle electrolysis anode solution after obtaining except ferrum.

2. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: in step (1), described ammonia chloride Concentration is 50～200g/L, and nickel ion concentration is 5～80g/L, and copper ion concentration is 1～5g/L, iron concentration be 0.05～ 1g/L, nickel sulfide concentration is 1～10g.

3. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1 or 2, it is characterised in that: in step (1), temperature model Enclosing is 40～60 DEG C, and magnetic agitation rotating speed is 400～600r/min, and mixing time is 20～80min.

4. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: in step (2), ammonia concn is 50～250g/L.

5. the impurity removal process of the nickle electrolysis anode solution as described in claim 1 or 4, it is characterised in that: in step (2), during stirring Between be 3～10min.

6. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: described technique by step (1)～ (2) composition.