CN113125430A - Method for measuring cyanide concentration in antimony-containing gold ore cyanidation leaching process - Google Patents
Method for measuring cyanide concentration in antimony-containing gold ore cyanidation leaching process Download PDFInfo
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- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 43
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 26
- 239000010931 gold Substances 0.000 title claims abstract description 26
- 238000002386 leaching Methods 0.000 title claims abstract description 21
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 17
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 27
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000004448 titration Methods 0.000 claims abstract description 23
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 239000012086 standard solution Substances 0.000 claims abstract description 11
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 8
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 26
- 229910001961 silver nitrate Inorganic materials 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 5
- KIWUVOGUEXMXSV-UHFFFAOYSA-N rhodanine Chemical compound O=C1CSC(=S)N1 KIWUVOGUEXMXSV-UHFFFAOYSA-N 0.000 description 5
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052959 stibnite Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
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Abstract
The invention relates to the technical field of ion concentration detection, in particular to a method for measuring cyanide concentration in a cyanide leaching process of antimony-containing gold ore, which comprises the following steps: step one, ore pulp which is undergoing cyanidation is taken and filtered to obtain clear liquid 1; step two, gradually adding excessive solid Pb (NO) into the clear solution 1 obtained in the step one3)2Filtering to obtain clear liquid 2; step three, adding excessive solid NaOH into the clear liquid 2 obtained in the step two, and filtering to obtain a clear liquid 3; step four, taking a certain amount of clear liquid 3 obtained in the step three, adding ammonia water into the clear liquid, adding potassium iodide into the clear liquid, and using AgNO to prepare the potassium iodide solution3Titrating the standard solution, recording AgNO when light yellow precipitate appears in the solution as a titration end point3And the consumption of the standard solution is used for calculating the cyanide concentration in the ore pulp. The beneficial effects are that: the invention is realized by usingExcess Pb (NO)3)2Removal of S from pulp affecting titration2‑After which excess NaOH is added to remove Pb affecting the KI indicator2+The influence of impurity ions on the titration of the cyanide is eliminated, and the rapid real-time monitoring of the concentration of the cyanide can be realized.
Description
Technical Field
The invention relates to the technical field of ion concentration detection, in particular to a method for measuring cyanide concentration in a cyanide leaching process of antimony-containing gold ore.
Background
Because the cyaniding gold leaching has a series of advantages of simple operation method, low operation cost, high technological degree and the like, the cyaniding gold leaching is still the most widely used in the existing gold leaching technology at present.
During cyanide leaching of gold, cyanide is consumed by gold dissolution and some impurity elements. If the concentration of cyanide in the ore pulp is too low, the dissolution speed of gold in the cyanidation process is too slow, and the time for gold to reach a high leaching rate is too long; if the concentration of cyanide in the ore pulp is too high, the consumption of cyanide is excessive, the cost is increased, and the waste residue and the waste water after cyanidation are not easy to treat, so that the environmental problem is caused. Therefore, the cyanide concentration in the ore pulp needs to be monitored in real time so as to grasp the cyanide consumption situation at any time, and cyanide is supplemented in time, so that gold dissolution is in a proper state, and the cyanidation time and the cyanide consumption are reduced.
The conventional method for detecting the cyanide concentration mainly detects the concentration of CN < - > in a solution, and the common methods are as follows: distillation, silver nitrate titration, rhodanine, and the like. The distillation method requires a long detection time, about 1-2 hours, which cannot achieve the purpose of rapid measurement, and is therefore not suitable for process control analysis; the silver nitrate method and the rhodanine method can quickly measure the concentration of free CN & lt- & gt within a few minutes, the basic principles are approximately the same, the difference is that the solution color at the end point of titration is different, the silver nitrate method shows milky yellow, and the rhodanine shows light red.
However, both the silver nitrate method and the rhodanine method are only suitable for rapidly determining free cyanide in a cyaniding process of oxidized ores with simple components, and when the ore pulp contains other ion components which can generate a coordination reaction or a precipitation reaction with silver ions, the detection result is affected, so that the condition that the titration end point cannot be observed and determined and the detection is inaccurate is caused.
In the process of cyaniding and leaching gold from antimony-containing gold ore, stibnite (Sb) is used2S3) In the alkaline cyanidation process, oxidation and dissolution easily occur, so that a large amount of S is generated2-Ions enter the solution phase, Ag in the standard titration solution during titration+Will take precedence over S2-The reaction generates a brownish red precipitate which consumes Ag+This will result in titration of the consumed Ag+Too much, the measured concentration deviation of cyanide is very large; also, Ag produced during the titration process2The S precipitate is brownish red, and the color development of the subsequent titration end point is covered no matter in the silver nitrate method or the rhodanine method, so that the titration end point cannot be observed.
If the method of firstly precipitating sulfur ions by using silver nitrate and then measuring the cyanide concentration after filtering is adopted, because excessive silver nitrate must be added firstly, the amount of subsequently dropwise adding silver nitrate titration solution is reduced, so that the detection result is low, a large amount of silver nitrate reagent is consumed, and the detection cost is greatly increased.
In the existing cyanide concentration detection technology, no better solution is provided for the phenomenon. Therefore, it is necessary to find a method for measuring the concentration of cyanide in the cyaniding and leaching process of the antimony-containing gold ore.
Disclosure of Invention
In order to solve the above problems, embodiments of the present invention provide a method for determining a cyanide concentration in a cyanide leaching process of an antimony-containing gold ore.
The purpose of the invention is realized as follows:
a method for measuring cyanide concentration in a cyanide leaching process of antimony-containing gold ore comprises the following steps:
step one, ore pulp which is undergoing cyanidation is taken and filtered to obtain clear liquid 1;
step two, gradually adding solid Pb (NO) into the clear liquid 1 obtained in the step one3)2Removal of S affecting the titration2-With Pb (NO)3)2The PbS gray-black precipitate is generated firstly when the PbS is added into the solution, and clear liquid 2 is obtained after filtration;
step three, adding excessive solid NaOH into the clear liquid 2 obtained in the step two to generate Pb (OH)2Removing excess Pb added in the previous step2+Filtering to obtain clear liquid 3;
step four, taking a certain amount of clear liquid 3 obtained in the step three, adding ammonia water into the clear liquid, adding potassium iodide into the clear liquid, and using AgNO to prepare the potassium iodide solution3Titrating the standard solution, recording AgNO when light yellow precipitate appears in the solution as a titration end point3And the consumption of the standard solution is used for calculating the cyanide concentration in the ore pulp.
Preferably, Pb (NO) in step two3)2Was added in excess until ashless black precipitate appeared.
Preferably, the NaOH is added in excess in step three until no white precipitate appears.
The embodiment of the invention has the beneficial effects that: the invention is realized by using excess Pb (NO)3)2Removal of S from pulp affecting titration2-After which excess NaOH is added to remove Pb affecting the KI indicator2+After the two steps of operation, the influence of the heteroatom on the cyaniding titration can be eliminated, and the real-time monitoring of the cyanide concentration can be realized.
Drawings
FIG. 1 is a schematic flow chart of a method for determining cyanide concentration in a cyanide leaching process of antimony-containing gold ore provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in figure 1, the method for measuring the cyanide concentration in the cyaniding leaching process of the antimony-containing gold ore comprises the following steps:
step one, 50ml of ore pulp undergoing cyanidation is taken and filtered to obtain clear liquid 1;
step two, gradually adding solid Pb (NO) into the clear liquid 1 obtained in the step one3)2Removal of S affecting the titration2-With Pb (NO)3)2The addition of (2) will generate a gray black PbS precipitate first, and an excessive amount of Pb (NO) will be added3)2Formation of white Pb (OH)2Precipitating, and filtering to obtain clear liquid 2;
ksp (pbs) 9 × 10 is known-29，Ksp(Pb(OH)2)＝1×10-16From this, it can be seen that when the pH of the slurry is 11, C is measured(OH-)When Pb (OH) is formed, the ratio is 0.001mol/L2Precipitation, then C(Pb2+)＝1×10-10mol/L, C in solution(S2-)＝9×10-19mol/L, can be regarded as complete removal. At this point in the solution:
Pb2++S2-→PbS↓ Pb2+2OH-→Pb(OH)2step III, adding excessive solid NaOH into the clear liquid 2 obtained in the step II to generate Pb (OH)2Removing excess Pb added in the previous step2+Filtering to obtain clear liquid 3;
step four, taking 10ml of clear liquid 3 obtained in the step three, adding 5 drops of ammonia water with the concentration of 1:1, adding 5 drops of 5% potassium iodide, and using the mass concentration of 1.734X 10-3g/ml AgNO3Titrating the standard solution, recording AgNO when light yellow precipitate appears in the solution as a titration end point3And the consumption of the standard solution is used for calculating the cyanide concentration in the ore pulp.
Ksp (agi) ═ 8.3 × 10 is known-17Kho (Ag (CN)2 -)＝1.26×1021The accompanying AgNO is known3Added dropwise, at which point the following reaction takes place:
Ag++2CN-→Ag(CN)2 - Ag++I-→AgI↓
with AgNO3Addition of Standard solution, Ag+First with CN-Complex reaction to generate Ag (CN)2 -When CN-When consumed, Ag+And I-AgI precipitate was formed by binding to reach the titration end point.
It is known that 5 drops of 5% potassium iodide were added to 10ml of the clear solution 3, and C in the solution was roughly estimated(I-)Not more than 0.0075mol/L, so that C in the solution(Ag+)>1.107×10-14At mol/L, a precipitate is generated to reach the titration end point.
It is known that 10ml of clear solution 3, AgNO, is taken3The mass concentration of the standard solution is 1.734X 10-3g/ml, if 8ml of AgNO is consumed3The mass concentration of sodium cyanide in the standard solution in this case can be calculated by the following equation.
Mass concentration of sodium cyanide AgNO3Mass concentration of AgNO3Consumption volume/relative molecular mass × 2 × relative molecular mass of sodium cyanide/volume of clear solution × 100% ═ 1.734 × 10-3×8/170×2×49/10＝0.0008g/ml。
Comparative experiment
Comparative experiments set up 4 groups, all performed as follows: firstly, the antimony-containing gold ore is ground to be more than 90 percent of minus 200 meshes, then the mass concentration of the ore pulp is adjusted to be 40 percent, the caustic soda is added to adjust the pH value of the ore to be between 10 and 11, then the ore pulp is oxidized and stirred for 2 to 3 hours, and when a large amount of S is dissolved in the ore pulp at the moment2-Adding a certain amount of cyanide, stirring for 20-30 seconds, immediately sampling and filtering to obtain a cyanide solution.
The comparison calculation method comprises the following steps: according to the specific gravity of the antimony-containing gold ore, the mass concentration of the ore pulp, the volume of the ore pulp and the mass of the added cyanide, the theoretical mass concentration of cyanide in the cyanide solution can be calculated.
The experiment group tests totally comprise 4 groups, and are respectively in one-to-one correspondence with the 4 groups of comparative tests, namely 4 embodiments: cyanide leaching tests are carried out on different antimony-containing gold ores, and the content of cyanide in the leaching solution is analyzed according to the method in the leaching process and is compared with the theoretical content of cyanide.
TABLE 1
The analytical comparison results are as follows: as can be seen from the comparison results in Table 1, under the conditions of different concentrations of the antimony-containing gold ore and the cyanide, the cyanide concentration value measured by the method of the invention is basically consistent with the theoretical cyanide content, and the error is extremely small, which indicates that the method has good adaptability and accuracy.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (3)
1. A method for measuring cyanide concentration in a cyanide leaching process of antimony-containing gold ore is characterized by comprising the following steps:
step one, ore pulp which is undergoing cyanidation is taken and filtered to obtain clear liquid 1;
step two, gradually adding solid Pb (NO) into the clear liquid 1 obtained in the step one3)2Removal of S affecting the titration2-With Pb (NO)3)2The PbS gray-black precipitate is generated firstly when the PbS is added into the solution, and clear liquid 2 is obtained after filtration;
step three, adding excessive solid NaOH into the clear liquid 2 obtained in the step two to generate Pb (OH)2Removing excess Pb added in the previous step2+Filtering to obtain clear liquid 3;
step four, taking a certain amount of clear liquid 3 obtained in the step three, adding ammonia water into the clear liquid, adding potassium iodide into the clear liquid, and using AgNO to prepare the potassium iodide solution3Titrating the standard solution, recording AgNO when light yellow precipitate appears in the solution as a titration end point3And the consumption of the standard solution is used for calculating the cyanide concentration in the ore pulp.
2. The method for determining cyanide concentration in the cyanidation leaching process of antimony-containing gold ore according to claim 1, wherein Pb (NO) is contained in the second step3)2Was added in excess until ashless black precipitate appeared.
3. The method for determining the cyanide concentration in the cyanidation leaching of the antimony-containing gold ore according to claim 1, characterized in that NaOH is added in excess in the third step until no white precipitate appears.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117247196A (en) * | 2023-11-07 | 2023-12-19 | 湖南省核地质调查所 | Method and system for removing antimony ions in water |
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2021
- 2021-04-19 CN CN202110419682.XA patent/CN113125430A/en active Pending
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117247196A (en) * | 2023-11-07 | 2023-12-19 | 湖南省核地质调查所 | Method and system for removing antimony ions in water |
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Application publication date: 20210716 |