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Method for Determination of Chloride Ion Content in Copper Electrolyte

A technology of chloride ion content and copper electrolyte, applied in the direction of material electrochemical variables, etc., can solve the problems of absorbance interference deviation, large deviation between measurement results and actual values, long operation time, etc., and achieve high accuracy and precision. The potential jump point is obvious, ensuring the effect of reliable recovery

Active Publication Date: 2017-10-17
铜陵有色金属集团股份有限公司
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Problems solved by technology

[0003] The assay method of chloride ion content in the traditional copper electrolyte mainly contains two kinds: one, potassium thiocyanate titration method, concrete steps are first the chloride ion in the copper electrolyte and silver nitrate generate insoluble silver chloride precipitation, Then use sulfuric acid to dissolve the separated silver chloride into silver sulfate, use ferric nitrate as indicator, and titrate silver with potassium thiocyanate standard titration solution to calculate the content of chloride ions, but because the copper electrolyte itself has a deep The blue color will affect the judgment of the titration end point, so the accuracy of the chloride ion content measured by this method is low, and the operation time of this method is long, and the process is cumbersome; 2. Silver chloride turbidity method, the specific steps are Silver nitrate is added to the solution, so that the chloride ions in the copper electrolyte react with silver nitrate to produce fine-grained white silver chloride precipitates, which are low in content and will be suspended in the solution to form a colloidal solution. Absorbance, thereby calculating the content of chloride ions, but the stability of the silver chloride suspension is poor at room temperature, and the color of each batch of copper electrolyte is different due to the difference in copper content, resulting in interference deviation of absorbance, not only In this way, using this method also needs to establish a standard curve, etc., resulting in too long operation time
[0004] In view of the technical defects in the above-mentioned existing technologies, in order to improve the measurement efficiency, some enterprises have adopted the potentiometric titration method to measure the chloride ion content in the copper electrolyte, but the temperature of the copper electrolyte under production control is about 60°C. The sampling temperature, pipetting temperature, and titration temperature in the process are not at the same level, resulting in poor reproducibility of the analysis results. In addition, in order to obtain high-quality cathode copper with a dense structure, smooth surface, and low impurity content, copper mining companies will use copper electrolyte Add appropriate amount of additives, such as gelatin, thiourea, avaton, etc., the addition of these additives, especially the addition of thiourea, will affect the stability of the results of the determination of chloride ion content by potentiometric titration, resulting in a large deviation between the measurement results and the actual value

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  • Method for Determination of Chloride Ion Content in Copper Electrolyte
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  • Method for Determination of Chloride Ion Content in Copper Electrolyte

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: the mensuration of chloride ion content in copper electrolytic solution

[0019] a. Add the silver nitrate standard solution with a concentration of 0.01mol / L to the reagent bottle of the potentiometer;

[0020] b. Add 10ml of copper electrolyte and 2ml of isopropanol to a beaker with a capacity of 100ml, add water to make the volume to 50ml, insert the silver composite electrode and titration head into the solution to be tested in the beaker, control the pipetting temperature and titration solution The temperature is 25°C-28°C, and the stirring speed is 625rpm;

[0021] c. Titrate the silver nitrate standard solution in the reagent bottle into the beaker, and record the volume v of the silver nitrate standard solution corresponding to the titration consumption during the potential jump 0 According to the formula to calculate the content of chloride ions in the copper electrolyte, 5 groups were measured using the above method conditions, and the results s...

Embodiment 2

[0022] Embodiment 2: the mensuration of chloride ion content in copper electrolytic solution

[0023] a. Add the silver nitrate standard solution with a concentration of 0.01mol / L to the reagent bottle of the potentiometer;

[0024] b. Add 15ml of copper electrolyte and 3ml of isopropanol to a beaker with a capacity of 100ml, add water to make the volume to 50ml, insert the silver composite electrode and titration head into the solution to be tested in the beaker, control the temperature of the pipetting and the volume of the titration solution The temperature is 15°C-18°C, and the stirring speed is 625rpm;

[0025] c. Titrate the silver nitrate standard solution in the reagent bottle into the beaker, and record the volume v of the silver nitrate standard solution corresponding to the titration consumption during the potential jump 0 , according to the formula to calculate the content of chloride ions in the copper electrolyte, using the above method conditions to measure 5 g...

Embodiment 3

[0026] Embodiment 3: the mensuration of chloride ion content in copper electrolytic solution

[0027] a. Add the silver nitrate standard solution with a concentration of 0.01mol / L to the reagent bottle of the potentiometer;

[0028] b. Add 20ml of copper electrolyte and 4ml of isopropanol to a beaker with a capacity of 100ml, add water to make the volume to 50ml, insert the silver composite electrode and titration head into the solution to be tested in the beaker, and control the temperature of pipetting and titration of the solution. The temperature is 20°C-23°C, and the stirring speed is 625rpm;

[0029] c. Titrate the silver nitrate standard solution in the reagent bottle into the beaker, and record the volume v of the silver nitrate standard solution corresponding to the titration consumption during the potential jump 0 According to the formula to calculate the content of chloride ions in the copper electrolyte, 5 groups were measured using the above method conditions, an...

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Abstract

The invention discloses a method for quickly and reliably measuring the content of chloride ions in a copper electrolyte, the steps are as follows: add silver nitrate standard solution with a concentration of 0.005-0.01mol / L to a reagent bottle of a potentiometer; b, according to 3- Add copper electrolyte and isopropanol to the beaker in turn at a volume ratio of 7:1, add water to 50-60mL, insert the silver composite electrode and titration head into the solution to be tested in the beaker, and the stirring speed is 620-630rpm; c, Drop the silver nitrate standard solution into the beaker, record the volume of the silver nitrate standard solution corresponding to the titration when the potential jumps, and calculate the content of chloride ions in the copper electrolyte according to the formula. In the present invention, isopropanol is added to the solution to be tested, so that the potential jump point obtained by potentiometric titration is obvious, and the measured potential is stable and repeatable, thereby ensuring the accuracy and precision of the calculated chloride ion content in the copper electrolyte. High precision, providing accurate and reliable guiding data for the actual production of copper mining enterprises, thereby ensuring the reliable recovery of precious metals and the output of electrolytic copper.

Description

technical field [0001] The invention relates to the technical field of metallurgical analysis, in particular to a method for determining the content of chloride ions in a copper electrolyte. Background technique [0002] In the prior art, copper mining enterprises generally use the prepared blister copper to refine pure copper by electrolysis. When refining copper by electrolysis, a mixed solution of sulfuric acid and copper sulfate is used as the copper electrolyte. In the electrolysis process, it is necessary to add an appropriate amount of chloride ions to the copper electrolyte. The purpose is not only to realize the recovery of the precious metal silver in the copper electrolyte, but also to prevent anode passivation, thereby facilitating the generation of electrolytic copper and improving the efficiency of electrolysis. Copper production. However, when the content of chloride ions in the copper electrolyte is low, the reaction between chloride ions and silver ions wil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/42
Inventor 史静钱庆长余晶晶周颖徐庆红
Owner 铜陵有色金属集团股份有限公司
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