Method for digesting solid impurity elements of lead, zinc and selenium in nickel electrolytic solution
阅读说明：本技术 一种消解镍电解溶液中的固体杂质元素铅、锌、硒的方法 (Method for digesting solid impurity elements of lead, zinc and selenium in nickel electrolytic solution ) 是由 周通 冯建华 郭勇 郑军福 卢晓锋 苏兰伍 张峰瑞 李亦婧 张四增 宛顺磊 刘军 于 2020-05-20 设计创作，主要内容包括：本发明公开了一种消解镍电解溶液中的固体杂质元素铅、锌、硒的方法,包括以下步骤：将镍电解溶液中的固体杂质用稀盐酸溶液、去离子水洗涤后干燥；向干燥后的镍电解溶液中的固体杂质中加入含有还原剂的有机弱酸溶液,得到混合物料；还原剂为水合肼、盐酸羟胺中的一种或两种,有机弱酸为甲酸、醋酸、丙酸中的一种或几种；将混合物料在50℃-80℃的条件下搅拌反应0.2h-1h。本发明方法与强酸消解方法不同,无需借助超声助溶、无赶酸操作,反应时间短,能够作为该类固体杂质消解的新方法。(The invention discloses a method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution, which comprises the following steps: washing solid impurities in the nickel electrolytic solution with a dilute hydrochloric acid solution and deionized water, and drying; adding an organic weak acid solution containing a reducing agent into solid impurities in the dried nickel electrolytic solution to obtain a mixed material; the reducing agent is one or two of hydrazine hydrate and hydroxylamine hydrochloride, and the organic weak acid is one or more of formic acid, acetic acid and propionic acid; the mixed materials are stirred and react for 0.2h to 1h at the temperature of 50 ℃ to 80 ℃. The method is different from a strong acid digestion method, does not need to be assisted by ultrasonic and does not need acid dispelling operation, has short reaction time, and can be used as a novel method for digesting the solid impurities.)
1. A method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution is characterized by comprising the following steps:
step (1): washing solid impurities in the nickel electrolytic solution with a dilute hydrochloric acid solution and deionized water, and drying;
step (2): adding an organic weak acid solution containing a reducing agent into solid impurities in the dried nickel electrolytic solution to obtain a mixed material; the reducing agent is one or two of hydrazine hydrate and hydroxylamine hydrochloride, and the organic weak acid is one or more of formic acid, acetic acid and propionic acid;
and (3): the mixed materials are stirred and react for 0.2h to 1h at the temperature of 50 ℃ to 80 ℃.
2. The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution according to claim 1, wherein the nickel electrolytic solution is a mixed solution of a nickel sulfate solution and a nickel chloride solution.
3. The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution according to claim 2, wherein the solid impurity elements in the nickel electrolytic solution are collected by a double-pipe filter, and the aperture of a filter cloth of the double-pipe filter is 1 um.
4. The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution according to claim 1, wherein in the step (1), the solid impurity in the nickel electrolytic solution is washed three times with a dilute hydrochloric acid solution with a pH of 4.0-5.5 and deionized water, and then dried, and the drying process conditions are as follows: the drying temperature is 80-100 ℃, and the drying time is 8-10 h.
5. The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution according to claim 1, wherein the concentration of the reducing agent in the step (2) is 0.01M-0.2M; the concentration of the organic weak acid solution is 30-60%.
Technical Field
The invention belongs to the technical field of chemical dissolution, and particularly relates to a method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution.
Background
Nickel electrolytic solutions are important electrolytes for electrolytic nickel production. The distinction according to the type of anion can be divided into sulfate Systems (SO)4 2-) Chlorine system (Cl)-) And mixed systems, which are electrolytes formulated with a certain sulfate/chloride ratio, are the most common electrolytic systems. The mixed acid system can obtain the standard nickel electrolyte suitable for electrolytic nickel production through sequentially removing iron (Fe), copper (Cu) and cobalt (Co) plasmas. In the impurity removal process, fine solid impurities can penetrate through the filter cloth and enter the solution to influence the quality of the electrolyteFurther influencing the quality of the electrolytic nickel. Therefore, the understanding of the state of the nickel electrolytic solution has important significance for monitoring and controlling the production conditions of electrolytic nickel and ensuring the quality of products. The content of metallic or non-metallic impurity elements such as lead (Pb), zinc (Zn), selenium (Se) and the like in the electrolytic nickel not only affects the quality of the electrolytic nickel, but also affects the performance of the nickel. Through analysis of solid impurity elements in the nickel electrolyte, the quality of the electrolyte and the quality of finished nickel can be indirectly evaluated. The traditional solid digestion method generally adopts strong inorganic acid (such as hydrochloric acid, nitric acid, hydrofluoric acid and aqua regia) to dissolve and digest the solid, the solution after digestion is heated to remove acid, and dilute inorganic acid with certain concentration is used for preparing the solution suitable for the detection of mass spectrometry (GB/T6041-. The traditional solid digestion method has the problems of long time consumption, more equipment investment, complicated steps and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution, which is simple, convenient to operate and short in time consumption.
The invention adopts the following technical scheme:
a method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution is characterized by comprising the following steps:
step (1): washing solid impurities in the nickel electrolytic solution with a dilute hydrochloric acid solution and deionized water, and drying;
step (2): adding an organic weak acid solution containing a reducing agent into solid impurities in the dried nickel electrolytic solution to obtain a mixed material; the reducing agent is one or two of hydrazine hydrate and hydroxylamine hydrochloride, and the organic weak acid is one or more of formic acid, acetic acid and propionic acid;
and (3): the mixed materials are stirred and react for 0.2h to 1h at the temperature of 50 ℃ to 80 ℃.
The method for digesting solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution is characterized in that the nickel electrolytic solution is a mixed solution composed of a nickel sulfate solution and a nickel chloride solution.
The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution is characterized in that the solid impurities in the nickel electrolytic solution are collected by a double-pipe filter, and the aperture of filter cloth of the double-pipe filter is 1 um.
The method for digesting the solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution is characterized in that in the step (1), the solid impurity in the nickel electrolytic solution is washed for three times by a dilute hydrochloric acid solution with the pH value of 4.0-5.5 and deionized water respectively, and then dried, and the drying process conditions are as follows: the drying temperature is 80-100 ℃, and the drying time is 8-10 h.
The method for digesting solid impurity elements of lead, zinc and selenium in the nickel electrolytic solution is characterized in that the concentration of the reducing agent in the step (2) is 0.01M-0.2M; the concentration of the organic weak acid solution is 30-60%.
The invention has the beneficial technical effects that: the invention applies the weak organic acid to the analysis of solid impurity components in the nickel electrolytic solution, not only can shorten the digestion time in the sample detection process, but also has low price of equipment required for digestion, simple operation method and easy grasp by workers. Meanwhile, the organic weak acid is a monodentate ligand, and the application of the organic weak acid is beneficial to improving the solubility of the metal elements (Pb and Zn) to be detected and enhancing the reliability of analysis data. The method is different from a strong acid digestion method, does not need to be assisted by ultrasonic and does not need acid dispelling operation, has short reaction time, and can be used as a novel method for digesting the solid impurities.
Detailed Description
The invention discloses a method for digesting solid impurity elements of lead, zinc and selenium in a nickel electrolytic solution, which comprises the following steps: step (1): and washing solid impurities in the nickel electrolytic solution with a dilute hydrochloric acid solution and deionized water, and drying, wherein the solid-liquid mass ratio of the solid impurities to the dilute hydrochloric acid solution is 0.25-0.5, and the solid-liquid mass ratio of the solid impurities to the deionized water is 0.25-0.5. Preferably, the solid impurities in the nickel electrolytic solution are washed three times with a dilute hydrochloric acid solution with a pH of 4.0-5.5 and deionized water, and then dried, wherein the drying process conditions are as follows: drying for 8-10 h in a forced air drying oven at 80-100 ℃. The nickel electrolytic solution is sulfuric acidNickel solution and nickel chloride solution. The solid impurities in the nickel electrolytic solution are mainly a mixture of nickel, cobalt, manganese and iron. Solid impurities in the nickel electrolytic solution are solid insoluble substances collected by a sleeve pipe precision filter, and the aperture of filter cloth of the sleeve pipe precision filter is 1 um. Step (2): adding an organic weak acid solution containing a reducing agent into solid impurities in the dried nickel electrolytic solution to obtain a mixed material; the reducing agent is hydrazine hydrate (N)2H4·H2O), hydroxylamine hydrochloride (NH)2OH & HCl), organic weak acid is formic acid (HCO)2H) Acetic acid (AcOH), propionic acid (EtCO)2H) One or more of the above; the concentration of the reducing agent is 0.01M-0.2M; the concentration of the organic weak acid solution is 30-60%. And (3): and (3) carrying out magneton stirring reaction on the mixed material at the temperature of 50-80 ℃ for 0.2-1 h, wherein the solution is light brown after the reaction and basically no solid remains. And detecting the contents of lead, zinc and selenium in the solution by ICP-MS according to GB/T6041-2002.
The chemical reaction equation involved in the digestion process of the solid impurities in the nickel electrolytic solution is as follows:
Ni(OH)2+2RCO2H＝Ni(RCO2)2+2H2O
4Fe(OH)3+8RCO2H+N2H4·H2O＝4Fe(RCO2)2+13H2O+N2↑
2Fe(OH)3+2RCO2H+2NH2OH·HCl＝Fe(RCO2)2+FeCl2+8H2O+N2↑
4Co(OH)3+8RCO2H+N2H4·H2O＝4Co(RCO2)2+13H2O+N2↑
2Co(OH)3+2RCO2H+2NH2OH·HCl＝Co(RCO2)2+CoCl2+8H2O+N2↑
MnO2+2RCO2H+N2H4·H2O＝Mn(RCO2)2+3H2O+N2↑
MnO2+2NH2OH·HCl＝MnCl2+4H2O+N2↑
PbCO3+2RCO2H＝Pb(RCO2)2+H2O+CO2↑
Pb3(OH)2(CO3)2+6RCO2H＝3Pb(RCO2)2+4H2O+2CO2↑
2Pb2O3+8RCO2H+N2H4·H2O＝4Pb(RCO2)2+7H2O+N2↑
Pb2O3+2RCO2H+2NH2OH·HCl＝Pb(RCO2)2+5H2O+N2↑+PbCl2
ZnCO3+2RCO2H＝Zn(RCO2)2+H2O+CO2↑
Zn3(OH)2(CO3)2+6RCO2H＝3Zn(RCO2)2+4H2O+2CO2↑
wherein, RCO2H represents weak organic acid, and R is H, Me or Et.
Selenium is mainly selenious acid (SeO)3 2-) And hydrogen selenite (HSeO)3 -) The corresponding acid radical negative ions gradually enter a solution state along with the dissolution of solid dissolved matters in the solid granular slag through form adsorption.
The invention is further illustrated by the following specific examples.
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