CN118067646A - Bivalent copper ion detection method for influencing molybdenum production - Google Patents

Bivalent copper ion detection method for influencing molybdenum production Download PDF

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CN118067646A
CN118067646A CN202410407660.5A CN202410407660A CN118067646A CN 118067646 A CN118067646 A CN 118067646A CN 202410407660 A CN202410407660 A CN 202410407660A CN 118067646 A CN118067646 A CN 118067646A
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solution
copper
standard
sample
molybdenum
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付鑫盛
孟祥辉
李超
侯霞宝
池耀东
马英
乔雅静
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Inner Mongolia Guocheng Industrial Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Acoustics & Sound (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a bivalent copper ion detection method for influencing molybdenum production, which comprises the following steps: (1) mixing; (2) constant volume; (3) detecting; (4) calculating. The beneficial effects are that: the method for detecting the cupric ions influencing the production of the molybdenum is quick, simple and easy to operate, can accurately detect the content of the free cupric ions in the ore pulp sample, can effectively guide the addition amount of the medicament in the production process of the molybdenum, is used for precipitating the free cupric ions, reduces the free cupric ions in the ore pulp solution, and improves the quality of molybdenum concentrate products.

Description

Bivalent copper ion detection method for influencing molybdenum production
Technical field:
The invention belongs to the technical field of copper ion detection in a molybdenum production process, and particularly relates to a bivalent copper ion detection method for influencing molybdenum production.
The background technology is as follows:
At present, no technological method is disclosed for measuring free cupric ions in ore pulp in the molybdenum production process, and the existence of the free cupric ions in the ore pulp can change the electrical properties of the mineral surface and make the mineral surface hydrophilic. This hydrophilicity increases the contact area of some sulphide minerals with water, making separation of the sulphide minerals difficult; further affecting the flotation effect, resulting in high doping amount of the subsequent molybdenum concentrate and reduced product quality; at present, the common method for detecting the copper content in the molybdenum ore only is used, wherein copper ions of CuCO 3 in ore pulp are not free and have no influence on molybdenum production, so that the common method for detecting the copper content in the molybdenum ore cannot accurately guide the addition of medicaments in production, and no report about a free bivalent copper ion detection method in ore pulp in the molybdenum production process exists at present.
Therefore, the invention provides a bivalent copper ion detection method for influencing molybdenum production, which has accurate detection result and small error.
The invention comprises the following steps:
Therefore, the invention aims to provide a cupric ion detection method for influencing molybdenum production, which is accurate in detecting the content of free cupric ions in ore pulp samples, can effectively guide the addition amount of a medicament in the molybdenum production process, is used for precipitating the free cupric ions, reduces the free cupric ions in ore pulp solution, and improves the quality of molybdenum concentrate products.
The technical scheme of the invention discloses a bivalent copper ion detection method for influencing molybdenum production, which comprises the following steps:
(1) Mixing: mixing the ore pulp sample with distilled water according to a volume ratio of 1:2-5, adding the mixture into a turnover oscillator, and then adding pure iron beads; then vibrating, mixing and leaching for 30-90min, and then carrying out solid-liquid separation to obtain a sample solution; the cupric ions in the ore pulp sample can be fully separated from the solid and dissolved into the sample solution by adding the iron beads, so that the detection accuracy of the cupric ion content is greatly improved.
(2) Constant volume: and (3) transferring 200mL of the sample solution in the step (1), placing the sample solution in a 250mL volumetric flask, and diluting the sample solution to a scale with 2% hydrochloric acid solution to obtain a solution to be measured.
(3) And (3) detection: and (3) detecting the copper-containing quality of the solution to be detected in the step (2) by utilizing an atomic absorption spectrophotometry.
(4) And (3) calculating: calculating the bivalent copper ion content of the ore pulp sample in the step (1) through a calculation formula, and specifically:
Wherein M 1 is the copper-containing mass of the solution to be tested in step (3);
M 0 is the mass of the pulp sample in step (1);
V 0 is the volume of distilled water added during leaching in step (1);
V 1 is the volume of the sample solution in the pipetting step (1).
Further, the preparation method further comprises the steps of preparing a standard solution before the step (3):
a. Weighing 0.1000g of spectral pure copper (more than or equal to 99.99 percent) and placing the spectral pure copper into a 300mL beaker, adding 5mL of nitric acid solution with the concentration of 1.42g/mL, cooling after slightly heating to dissolve completely, then transferring all the solution into a 100mL volumetric flask, fixing the volume to a scale, and shaking uniformly to obtain mother solution;
b. c, placing 20mL of the mother solution in the step a into a 1000mL volumetric flask, diluting with 2% hydrochloric acid until the mother solution is uniformly shaken to obtain sub-standard solution;
c. And c, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of the sub standard solution in the step b, placing the sub standard solution in a group of 50mL volumetric flasks, diluting to a scale with 2% hydrochloric acid solution, and shaking uniformly to obtain the standard solution.
Further, the detecting in the step (3) specifically includes: and on the atomic absorption spectrophotometer, using oxygen-enriched air-acetylene flame, measuring the absorbance of 7 standard solutions and copper in the solution to be detected at the wavelength 324.7nm, establishing a standard curve of copper by the absorbance of 7 standard solutions and the known copper mass of the standard solutions, and then checking the copper mass of the solution to be detected by the absorbance of copper of the solution to be detected from the standard curve.
Furthermore, the standard curve is fitted and drawn by taking the copper-containing quality value of the known standard solution as an abscissa and the corresponding absorbance as an ordinate.
The invention has the advantages that:
The method for detecting the cupric ions influencing the production of the molybdenum is quick, simple and easy to operate, can accurately detect the content of the free cupric ions in the ore pulp sample, can effectively guide the addition amount of the medicament in the production process of the molybdenum, is used for precipitating the free cupric ions, reduces the amount of the free cupric ions in the ore pulp solution, and improves the quality of molybdenum concentrate products.
The specific embodiment is as follows:
The present invention will be described in further detail by way of examples.
Example 1: a method for detecting cupric ions affecting molybdenum production, comprising the steps of:
(1) Mixing: 500mL of ore pulp sample and 1000mL of distilled water are added into a turning oscillator, and then 3g of pure iron beads are added; then vibrating, mixing and leaching for 30min, and then carrying out solid-liquid separation to obtain a sample solution; free cupric ions in the ore pulp sample can be fully separated and dissolved from the solid into the sample solution in the shaking process by adding the iron beads, so that the detection accuracy of the cupric ion content is greatly improved.
(2) Constant volume: and (3) transferring 200mL of the sample solution in the step (1), placing the sample solution in a 250mL volumetric flask, and diluting the sample solution to a scale with 2% hydrochloric acid solution to obtain a solution to be measured.
Preparing a standard solution:
a. Weighing 0.1000g of spectral pure copper (more than or equal to 99.99 percent) and placing the spectral pure copper into a 300mL beaker, adding 5mL of nitric acid solution with the concentration of 1.42g/mL, cooling after slightly heating to dissolve completely, then transferring all the solution into a 100mL volumetric flask, fixing the volume to a scale, and shaking uniformly to obtain mother solution;
b. c, placing 20mL of the mother solution in the step a into a 1000mL volumetric flask, diluting with 2% hydrochloric acid until the mother solution is uniformly shaken to obtain sub-standard solution;
c. And c, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of the sub standard solution in the step b, placing the sub standard solution in a group of 50mL volumetric flasks, diluting to a scale with 2% hydrochloric acid solution, and shaking uniformly to obtain the standard solution.
(3) And (3) detection: measuring the absorbance of 7 standard solutions and copper in the solution to be measured in the step (2) at the wavelength 324.7nm by using oxygen-enriched air-acetylene flame on an atomic absorption spectrophotometer, and establishing a standard curve of copper by using the absorbance of 7 standard solutions and the copper-containing mass of the known standard solution, wherein the standard curve is fitted and drawn by taking the copper-containing mass value of the known standard solution as an abscissa and the corresponding absorbance as an ordinate; and then, checking the copper-containing quality of the solution to be tested according to the absorbance of the copper of the solution to be tested on a standard curve.
(4) And (3) calculating: calculating the bivalent copper ion content of the ore pulp sample in the step (1) through a calculation formula, and specifically:
Wherein M 1 is the copper-containing mass of the solution to be tested in step (3);
M 0 is the mass of the pulp sample in step (1);
V 0 is the volume of distilled water added during leaching in step (1);
V 1 is the volume of the sample solution in the pipetting step (1).
Example 2: a method for detecting cupric ions affecting molybdenum production, comprising the steps of:
(1) Mixing: 500mL of ore pulp sample and 1500mL of distilled water are added into a turning oscillator, and then 3g of pure iron beads are added; then vibrating, mixing and leaching for 60min, and then carrying out solid-liquid separation to obtain a sample solution; through adding the iron beads, bivalent copper ions in the ore pulp sample can be fully separated and dissolved from solids into a sample solution in the vibration process, so that the detection accuracy of the bivalent copper ion content is greatly improved.
(2) Constant volume: and (3) transferring 200mL of the sample solution in the step (1), placing the sample solution in a 250mL volumetric flask, and diluting the sample solution to a scale with 2% hydrochloric acid solution to obtain a solution to be measured.
Preparing a standard solution:
a. Weighing 0.1000g of spectral pure copper (more than or equal to 99.99 percent) and placing the spectral pure copper into a 300mL beaker, adding 5mL of nitric acid solution with the concentration of 1.42g/mL, cooling after slightly heating to dissolve completely, then transferring all the solution into a 100mL volumetric flask, fixing the volume to a scale, and shaking uniformly to obtain mother solution;
b. c, placing 20mL of the mother solution in the step a into a 1000mL volumetric flask, diluting with 2% hydrochloric acid until the mother solution is uniformly shaken to obtain sub-standard solution;
c. And c, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of the sub standard solution in the step b, placing the sub standard solution in a group of 50mL volumetric flasks, diluting to a scale with 2% hydrochloric acid solution, and shaking uniformly to obtain the standard solution.
(3) And (3) detection: measuring the absorbance of 7 standard solutions and copper in the solution to be measured in the step (2) at the wavelength 324.7nm by using oxygen-enriched air-acetylene flame on an atomic absorption spectrophotometer, and establishing a standard curve of copper by using the absorbance of 7 standard solutions and the copper-containing mass of the known standard solution, wherein the standard curve is fitted and drawn by taking the copper-containing mass value of the known standard solution as an abscissa and the corresponding absorbance as an ordinate; and then, checking the copper-containing quality of the solution to be tested according to the absorbance of the copper of the solution to be tested on a standard curve.
(4) And (3) calculating: calculating the bivalent copper ion content of the ore pulp sample in the step (1) through a calculation formula, and specifically:
Wherein M 1 is the copper-containing mass of the solution to be tested in step (3);
M 0 is the mass of the pulp sample in step (1);
V 0 is the volume of distilled water added during leaching in step (1);
V 1 is the volume of the sample solution in the pipetting step (1).
Example 3: a method for detecting cupric ions affecting molybdenum production, comprising the steps of:
(1) Mixing: 500mL of ore pulp sample and 2500mL of distilled water are added into a turning oscillator, and then 3g of pure iron beads are added; then vibrating, mixing and leaching for 30min, and then carrying out solid-liquid separation to obtain a sample solution; through adding the iron beads, bivalent copper ions in the ore pulp sample can be fully separated and dissolved from solids into a sample solution in the vibration process, so that the detection accuracy of the bivalent copper ion content is greatly improved.
(2) Constant volume: and (3) transferring 200mL of the sample solution in the step (1), placing the sample solution in a 250mL volumetric flask, and diluting the sample solution to a scale with 2% hydrochloric acid solution to obtain a solution to be measured.
Preparing a standard solution:
a. Weighing 0.1000g of spectral pure copper (more than or equal to 99.99 percent) and placing the spectral pure copper into a 300mL beaker, adding 5mL of nitric acid solution with the concentration of 1.42g/mL, cooling after slightly heating to dissolve completely, then transferring all the solution into a 100mL volumetric flask, fixing the volume to a scale, and shaking uniformly to obtain mother solution;
b. c, placing 20mL of the mother solution in the step a into a 1000mL volumetric flask, diluting with 2% hydrochloric acid until the mother solution is uniformly shaken to obtain sub-standard solution;
c. And c, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of the sub standard solution in the step b, placing the sub standard solution in a group of 50mL volumetric flasks, diluting to a scale with 2% hydrochloric acid solution, and shaking uniformly to obtain the standard solution.
(3) And (3) detection: measuring the absorbance of 7 standard solutions and copper in the solution to be measured in the step (2) at the wavelength 324.7nm by using oxygen-enriched air-acetylene flame on an atomic absorption spectrophotometer, and establishing a standard curve of copper by using the absorbance of 7 standard solutions and the copper-containing mass of the known standard solution, wherein the standard curve is fitted and drawn by taking the copper-containing mass value of the known standard solution as an abscissa and the corresponding absorbance as an ordinate; and then, checking the copper-containing quality of the solution to be tested according to the absorbance of the copper of the solution to be tested on a standard curve.
(4) And (3) calculating: calculating the bivalent copper ion content of the ore pulp sample in the step (1) through a calculation formula, and specifically:
Wherein M 1 is the copper-containing mass of the solution to be tested in step (3);
M 0 is the mass of the pulp sample in step (1);
V 0 is the volume of distilled water added during leaching in step (1);
V 1 is the volume of the sample solution in the pipetting step (1).
Comparative example 1: the overall detection method was the same as in example 2, except that mixing: 500mL of ore pulp sample and 1500mL of distilled water are added into a turning oscillator, mixed and leached for 60min under shaking, and then solid-liquid separation is carried out, so as to obtain sample solution.
Standard sample detection experiment: adopting 12 ore pulp samples of different ore types, wherein each sample is divided into 8 groups, wherein 4 groups of ore samples are respectively subjected to free cupric ion content detection by using the methods disclosed in examples 1-3 and comparative example 1 to obtain 4 groups of free cupric ion content values before addition of standard, and the other 4 groups are respectively added with 1mL of copper sulfate solution with the concentration of 5ug/mL, and then are respectively subjected to free cupric ion content detection by using the methods disclosed in examples 1-3 and comparative example 1 to obtain 4 groups of free cupric ion content values after addition of standard; the free cupric ion content values before the addition of the standard, which are detected by the corresponding method, are subtracted from the free cupric ion content values after the addition of the standard in the 4 groups, so that the detection value of cupric ions in the cupric sulfate solution is obtained; the specific results are shown in table 1 below:
TABLE 1 detection results of free cupric ions
From table 1, it can be seen that, in the molybdenum production process, pulp samples with different property categories are detected by standard adding tests under the same leaching condition, and the accuracy of examples 1-3 is over 94%, so that the detection method of the invention can fully meet the requirement of detecting free cupric ions in production, further can effectively guide the addition amount of the medicament in the molybdenum production process, is used for precipitating the free cupric ions, reduces the free cupric ions in pulp solution, and improves the quality of molybdenum concentrate products.
Meanwhile, the accuracy of the comparative example 1 is below 90%, which is far lower than the detection accuracy of the examples 1-3, so that the cupric ions in the ore pulp sample can be fully separated and dissolved from the solid into the sample solution in the vibration process of the added iron beads, and the detection accuracy of the cupric ion content is greatly improved.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that modifications and variations can be made without departing from the principles of the present invention, and such modifications and variations are to be regarded as being within the scope of the invention.

Claims (4)

1. A method for detecting cupric ions affecting molybdenum production, comprising the steps of:
(1) Mixing: mixing the ore pulp sample with distilled water according to a volume ratio of 1:2-5, adding the mixture into a turnover oscillator, and then adding pure iron beads; then vibrating, mixing and leaching for 30-90min, and then carrying out solid-liquid separation to obtain a sample solution;
(2) Constant volume: transferring 200mL of the sample solution obtained in the step (1), placing the sample solution in a 250mL volumetric flask, and diluting the sample solution to a scale with 2% hydrochloric acid solution to obtain a solution to be measured;
(3) And (3) detection: detecting the copper-containing quality of the solution to be detected in the step (2) by utilizing an atomic absorption spectrophotometer;
(4) And (3) calculating: calculating the bivalent copper ion content of the ore pulp sample in the step (1) through a calculation formula, and specifically:
Wherein M 1 is the copper-containing mass of the solution to be tested in step (3);
M 0 is the mass of the pulp sample in step (1);
V 0 is the volume of distilled water added during leaching in step (1);
V 1 is the volume of the sample solution in the pipetting step (1).
2. The method for detecting cupric ions affecting molybdenum production according to claim 1, further comprising preparing a standard solution prior to step (3):
a. Weighing 0.1000g of spectral pure copper (more than or equal to 99.99 percent) and placing the spectral pure copper into a 300mL beaker, adding 5mL of nitric acid solution with the concentration of 1.42g/mL, cooling after slightly heating to dissolve completely, then transferring all the solution into a 100mL volumetric flask, fixing the volume to a scale, and shaking uniformly to obtain mother solution;
b. c, placing 20mL of the mother solution in the step a into a 1000mL volumetric flask, diluting with 2% hydrochloric acid until the mother solution is uniformly shaken to obtain sub-standard solution;
c. And c, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of the sub standard solution in the step b, placing the sub standard solution in a group of 50mL volumetric flasks, diluting to a scale with 2% hydrochloric acid solution, and shaking uniformly to obtain the standard solution.
3. The method for detecting cupric ions affecting molybdenum production according to claim 2, wherein the step (3) of detecting specifically comprises: and on the atomic absorption spectrophotometer, using oxygen-enriched air-acetylene flame, measuring the absorbance of 7 standard solutions and copper in the solution to be detected at the wavelength 324.7nm, establishing a standard curve of copper by the absorbance of 7 standard solutions and the known copper mass of the standard solutions, and then checking the copper mass of the solution to be detected by the absorbance of copper of the solution to be detected from the standard curve.
4. A method for detecting cupric ions affecting molybdenum production according to claim 3, wherein said standard curve is a linear curve fitted and drawn with the copper-containing mass value of known standard solution as the abscissa and the corresponding absorbance as the ordinate.
CN202410407660.5A 2024-04-07 2024-04-07 Bivalent copper ion detection method for influencing molybdenum production Pending CN118067646A (en)

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