CN117107065A - Technological method for extracting gold from gold mud - Google Patents
Technological method for extracting gold from gold mud Download PDFInfo
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- CN117107065A CN117107065A CN202310925845.0A CN202310925845A CN117107065A CN 117107065 A CN117107065 A CN 117107065A CN 202310925845 A CN202310925845 A CN 202310925845A CN 117107065 A CN117107065 A CN 117107065A
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- gold
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- gold mud
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 239000010931 gold Substances 0.000 title claims abstract description 199
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 198
- 238000000034 method Methods 0.000 title claims abstract description 53
- 230000008569 process Effects 0.000 claims abstract description 37
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001914 filtration Methods 0.000 claims abstract description 28
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 28
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000010881 fly ash Substances 0.000 claims description 111
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 238000000227 grinding Methods 0.000 claims description 26
- 239000000395 magnesium oxide Substances 0.000 claims description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 23
- 229920001661 Chitosan Polymers 0.000 claims description 21
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 description 40
- 239000012535 impurity Substances 0.000 description 31
- 239000002245 particle Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 17
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000011133 lead Substances 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 229910052745 lead Inorganic materials 0.000 description 10
- 239000011701 zinc Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 229910052725 zinc Inorganic materials 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000010953 base metal Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000875 corresponding effect Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000005805 hydroxylation reaction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/06—Chloridising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
Abstract
The application belongs to the technical field of gold extraction, and particularly discloses a process method for extracting gold from gold mud. The method comprises the following steps: (1) Immersing gold mud into a nitric acid solution with the mass concentration of 35-45%, reacting for 2-3 hours at the temperature of 65-70 ℃, filtering for solid-liquid separation, and collecting filter residues; (2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 30-45min at the temperature of 75-80 ℃, then heating, reacting for 2-3h at the temperature of 95-98 ℃, filtering to perform solid-liquid separation, and collecting filtrate, wherein the mass ratio of the filter residue to the aqua regia is 1:2-5; (3) Adding a reducing agent into the filtrate obtained in the step (2), reacting for 2-3 hours at the temperature of 80-85 ℃ to obtain gold powder with the purity of more than 99.5%, washing, filtering, drying and smelting to obtain gold ingots. The application obtains gold powder with purity of more than 99.5 percent, and has simple operation and high gold extraction efficiency and purity.
Description
Technical Field
The application relates to the technical field of gold extraction, in particular to a process method for extracting gold from gold mud.
Background
Gold is a rare strategic metal, is widely applied to gold ornaments, money stores, electronics industry, modern communication, aerospace and other high-tech industries, and has higher application value. Gold is generally extracted from gold mud in gold ore, and the gold mud contains a large amount of noble metal silver and a large amount of metal impurity elements such as iron, copper, lead, zinc, nickel and the like besides gold noble metal, and in order to obtain gold ingots with better quality, impurity removal treatment is generally required before refining, and most of impurity metal elements in the gold mud are separated.
In the prior art, a sulfuric acid leaching method is generally adopted, concentrated sulfuric acid is used for leaching at a certain temperature, so that metals such as copper, zinc, nickel, silver and the like are dissolved to form sulfate, and gold is not dissolved in the concentrated sulfuric acid and remains in slag, so that the purpose of separating gold from other metals is achieved, but the operation method is more severe in reaction, more sulfur dioxide gas can be generated, the environment is polluted, the acid consumption is higher, and the method is not suitable for industrial production.
Disclosure of Invention
In order to solve the problems of severe gold extraction reaction and easy environmental pollution of generated sulfur dioxide gas in the sulfuric acid digestion method, the application provides a process method for extracting gold from gold mud.
The application provides a process method for extracting gold from gold mud, which adopts the following technical scheme:
a technological method for extracting gold from gold mud comprises the following steps:
(1) Immersing gold mud into a nitric acid solution with the mass concentration of 35-45%, reacting for 2-3 hours at the temperature of 65-70 ℃, filtering for solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 30-45min at the temperature of 75-80 ℃, then heating, reacting for 2-3h at the temperature of 95-98 ℃, filtering to perform solid-liquid separation, and collecting filtrate, wherein the mass ratio of the filter residue to the aqua regia is 1:2-5;
(3) Adding a reducing agent into the filtrate obtained in the step (2), reacting for 2-3 hours at the temperature of 80-85 ℃ to obtain gold powder with the purity of more than 99.5%, washing, filtering, drying and smelting to obtain gold ingots.
By adopting the technical scheme, in the step (1), the nitric acid solution is used for removing copper, iron, zinc and other base metals and silver in the gold mud, the copper, iron, zinc and other base metals and silver in the gold mud can react with nitric acid to generate fusible salts, and gold is insoluble in the nitric acid solution, so that impurities and gold are separated.
Treating the collected filter residue with aqua regia, reacting gold in the filter residue with the aqua regia to dissolve gold in the filter residue in the aqua regia, filtering, collecting filtrate, and separating gold from other impurities; in the step, the gold is heated in stages, firstly, the gold is reacted for a period of time at the temperature of 75-80 ℃ to enable most of gold to be dissolved in the aqua regia, then the temperature is raised, the aqua regia is further activated, the corrosion capacity of the aqua regia is enhanced, gold is further dissolved, and gold is dissolved as much as possible, so that the gold extraction efficiency and purity are improved.
And finally, adding a reducing agent into the filtrate, and separating the gold complex from impurities in the leaching solution by utilizing the selective reduction characteristic of the reducing agent on gold to reduce the gold complex from an ionic state to obtain gold powder with the purity of more than 99.5%, and drying and smelting the reduced gold powder to obtain gold ingots.
Preferably, the mass ratio of the gold mud to the nitric acid solution is 1:6-8.
By adopting the technical scheme, the ratio of the gold mud to the nitric acid solution is further limited within a certain range, so that the raw material saving and the maximization of the reaction with the gold mud are ensured, and impurities and gold are effectively separated.
Preferably, the reducing agent is one or more of sodium sulfite, oxalic acid and hydrazine hydrate.
By adopting the technical scheme, the reducing agent reduces metal ions into metal simple substance, so that gold with higher purity is obtained, the operation is simple, and the reaction time is saved.
Preferably, before step (1), the gold mud is pretreated, and the pretreatment comprises the following steps: dispersing gold mud in deionized water, adding a grinding aid, grinding, filtering, and drying to obtain pretreated gold mud; grinding aids include magnesium oxide, fly ash and silicones.
Through adopting above-mentioned technical scheme, use grinding aid to carry out preliminary treatment to gold mud, grind gold mud, obtain the gold mud that the dispersion is even, granule size is even, help the reaction of follow-up gold mud and nitric acid solution, the time of the reaction of saving, and the granule size of gold mud is unanimous moreover, improved gold mud and nitric acid solution reaction's efficiency, and then help copper, iron, zinc etc. base metal and silver in the gold mud can react with nitric acid fast, improved gold's extraction purity.
The magnesium oxide has stronger oxidation resistance, adsorption performance, wear resistance, corrosion resistance and sterilization performance, can be effectively mixed with the gold mud after being added into the gold mud, increases the grinding performance of the gold mud, reduces the grinding resistance of the gold mud and prevents aggregation of gold mud particles, and the organosilicon can improve the surface performance of the fly ash particles, thereby enhancing the wear resistance, corrosion resistance and oxidation resistance of the fly ash; the magnesium oxide can be adsorbed on the surface and in the pores of the fly ash particles, the specific surface area of the fly ash is increased, the surface of the fly ash particles can be coated by the organic silicon, and the magnesium oxide, the fly ash and the organic silicon are matched to further improve the oxidation resistance, wear resistance and corrosion resistance of the fly ash, so that the grinding between the follow-up grinding aid and the gold mud is facilitated, the friction force and the adhesion force between the gold mud particles are reduced, the activity of the gold mud particles is increased, and the reaction of the follow-up gold mud and the nitric acid solution is facilitated.
Preferably, the mass ratio of the magnesium oxide to the fly ash to the organosilicon is 0.1-0.3:1:0.06-0.08.
By adopting the technical scheme, the mass ratio of the magnesium oxide, the fly ash and the organic silicon is further limited within a certain range, the grinding aid with strong oxidation resistance, high wear resistance and strong corrosion resistance is obtained, the magnesium oxide, the fly ash and the organic silicon have a synergistic effect, the magnesium oxide is loaded on the surface and in the pores of the fly ash, the organic silicon coats the fly ash, the connectivity between the fly ash and the magnesium oxide is further increased, the corresponding performance of the fly ash is further enhanced, and then the dispersibility of the gold mud particles is improved.
Preferably, the mass ratio of the gold mud to the grinding aid is 1:0.3-0.6.
By adopting the technical scheme, the mass ratio of the gold mud to the grinding aid is further limited, gold mud particles with good dispersibility are obtained, further the subsequent reaction of the gold mud and the nitric acid solution is facilitated, raw materials are saved, the gold mud is ensured to be dispersed to the greatest extent, and the subsequent corresponding treatment process is facilitated.
Preferably, the fly ash is pretreated by: pulverizing and sieving the fly ash to obtain fly ash fine powder, soaking the fly ash fine powder in a sulfuric acid solution with the mass fraction of 15% for 1-3h, washing the fly ash fine powder with water, adding the fly ash fine powder into a silane coupling agent, stirring the fly ash fine powder for 1-3h at 80-90 ℃, adding chitosan, continuously stirring the chitosan, washing the fly ash fine powder with water, filtering and drying the fly ash fine powder to obtain the modified fly ash.
By adopting the technical scheme, the fly ash is treated by sulfuric acid, the sulfuric acid degrades the surface of the fly ash particles to a certain extent, the pore and hole number of the surface of the fly ash particles are increased, the specific surface area of the fly ash is further increased, then the silane coupling agent is used for grafting modification on the surface of the fly ash, so that the silane coupling agent and the fly ash are subjected to hydroxylation reaction, the surface activity of the fly ash is improved, the fly ash is mixed with chitosan, the chitosan is grafted on the surface of the fly ash by the silane coupling agent, the surface activity of the fly ash is further improved, the adsorptivity of the fly ash is enhanced, and the subsequent mixing of the fly ash and other components is facilitated.
Preferably, the mass ratio of the fly ash to the silane coupling agent to the chitosan is 1:2-5:0.06-0.09.
By adopting the technical scheme, the mass ratio of the fly ash, the silane coupling agent and the chitosan is further limited within a certain range, so that the fly ash with better adsorptivity and higher surface activity is obtained, the fly ash, the silane coupling agent and the chitosan have a synergistic effect, the silane coupling agent and the fly ash are subjected to crosslinking modification, and the chitosan and the silane coupling agent are grafted, so that the performance between the fly ash is improved, and the subsequent improvement of the corresponding performance of the fly ash as a grinding aid is facilitated.
Preferably, the mass ratio of the fly ash to the sulfuric acid solution is 1:3-6.
By adopting the technical scheme, the ratio of the fly ash to the sulfuric acid solution is further limited within a certain range, so that the raw material saving is ensured, the maximization of the fly ash treatment is ensured, and the surface of the fly ash is effectively treated.
Preferably, the stirring speed is 300-500r/min.
By adopting the technical scheme, the stirring speed is further limited, so that the fly ash and other components are uniformly mixed, and the completeness of the reaction is ensured.
In summary, the application has the following beneficial effects:
1. the application uses nitric acid solution to remove base metals such as copper, iron, zinc and the like and silver in gold mud, uses aqua regia to treat the collected filter residues, separates gold from other impurities, finally uses the selective reduction characteristic of reducing agent to gold to reduce gold complex from ion state to separate simple substance gold from the impurities in leaching solution, and obtains gold powder with purity of over 99.5%, and the gold powder after reduction is dried and smelted to obtain gold ingot.
2. According to the application, the grinding aid is used for preprocessing the gold mud, and the gold mud is ground to obtain the gold mud which is uniformly dispersed and uniform in particle size, so that the subsequent reaction of the gold mud and the nitric acid solution is facilitated, the reaction time is saved, the particle size of the gold mud is uniform, the reaction efficiency of the gold mud and the nitric acid solution is improved, the copper, iron, zinc and other base metals and silver in the gold mud can be further facilitated to react with nitric acid rapidly, and the extraction purity of gold is improved.
3. According to the application, the magnesium oxide can be adsorbed on the surfaces and in the pores of the fly ash particles, the specific surface area of the fly ash is increased, the surface of the fly ash particles can be coated by the organic silicon, and the magnesium oxide, the fly ash and the organic silicon are matched to further improve the oxidation resistance, wear resistance and corrosion resistance of the fly ash, so that the grinding between the subsequent grinding aid and the gold mud is facilitated, the friction force and the adhesion force between the gold mud particles are reduced, the activity of the gold mud particles is increased, and the subsequent reaction of the gold mud and the nitric acid solution is facilitated.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the examples and comparative examples are all commercially available; wherein the reducing agent is sodium sulfite.
Preparation example of pretreatment
PREPARATION EXAMPLE 1-1
Before the step (1), pretreating the gold mud, wherein the pretreatment comprises the following steps: dispersing 1kg of gold mud in 3L of deionized water, adding a grinding aid, grinding, filtering, and drying to obtain pretreated gold mud; the grinding aid comprises magnesium oxide, fly ash and organic silicon; wherein the mass ratio of the magnesium oxide to the fly ash to the organic silicon is 0.1:1:0.06; the mass ratio of the gold mud to the grinding aid is 1:0.3;
the fly ash is pretreated by the following steps: crushing and sieving 1kg of fly ash to obtain fly ash fine powder, soaking in 2L of sulfuric acid solution with the mass fraction of 15% for 2h, washing with water, adding into a silane coupling agent, stirring at 85 ℃ for 2h, adding chitosan, continuously stirring, washing with water, filtering, and drying to obtain modified fly ash; wherein the mass ratio of the fly ash to the silane coupling agent to the chitosan is 1:2:0.09; the mass ratio of the fly ash to the sulfuric acid solution is 1:6; the stirring rate was 500r/min.
PREPARATION EXAMPLES 1-2
The difference from preparation example 1-1 is that no magnesium oxide was added.
Preparation examples 1 to 3
The difference from preparation example 1-1 is that no silicone was added.
Preparation examples 1 to 4
The difference from preparation example 1-1 is that the mass ratio of magnesium oxide, fly ash and organosilicon is 0.3:1:0.08.
Preparation examples 1 to 5
The difference from preparation example 1-1 is that the mass ratio of magnesium oxide, fly ash and organosilicon is 0.5:1:0.02.
Preparation examples 1 to 6
The difference from preparation example 1-1 is that the mass ratio of the gold mud to the grinding aid is 1:0.6.
Preparation examples 1 to 7
The difference from preparation example 1-1 is that fly ash was not pretreated.
Preparation examples 1 to 8
The difference from preparation example 1-1 is that no silane coupling agent is added during the pretreatment of the fly ash.
Preparation examples 1 to 9
The difference from preparation example 1-1 is that chitosan is not added in the pretreatment process of the fly ash.
Preparation examples 1 to 10
The difference from preparation example 1-1 is that the mass ratio of fly ash, silane coupling agent and chitosan is 1:5:0.06.
Preparation examples 1 to 11
The difference from preparation example 1-1 is that the mass ratio of fly ash, silane coupling agent and chitosan is 1:7:0.01.
Preparation examples 1 to 12
The difference from preparation example 1-1 is that the mass ratio of fly ash to sulfuric acid solution is 1:3.
Preparation examples 1 to 13
The difference from preparation example 1-1 is that the stirring rate was 300r/min.
Examples
Example 1
A technological method for extracting gold from gold mud comprises the following steps:
(1) Immersing 0.8kg of gold mud into a nitric acid solution with the mass concentration of 35%, reacting for 2 hours at the temperature of 70 ℃, filtering to perform solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 30min at the temperature of 80 ℃, then heating, reacting for 2h at the temperature of 98 ℃, wherein the mass ratio of the filter residue to the aqua regia is 1:5, filtering, performing solid-liquid separation, and collecting filtrate;
(3) Adding 0.5kg of reducing agent into the filtrate obtained in the step (2), reacting for 2 hours at the temperature of 85 ℃ to obtain gold powder with the purity of 99.5%, washing, filtering, drying and smelting to obtain gold ingots; wherein the mass ratio of the gold mud to the nitric acid solution is 1:8.
Example 2
A technological method for extracting gold from gold mud comprises the following steps:
(1) Immersing 0.9kg of gold mud into a nitric acid solution with the mass concentration of 45%, reacting for 3 hours at the temperature of 65 ℃, filtering to perform solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 45min at the temperature of 75 ℃, then heating, reacting for 3h at the temperature of 95 ℃, wherein the mass ratio of the filter residue to the aqua regia is 1:2, filtering, performing solid-liquid separation, and collecting filtrate;
(3) Adding 0.4kg of reducing agent into the filtrate obtained in the step (2), reacting for 3 hours at the temperature of 80 ℃ to obtain gold powder with the purity of 99.5%, washing, filtering, drying and smelting to obtain gold ingots; wherein the mass ratio of the gold mud to the nitric acid solution is 1:6.
Example 3
The process for extracting gold from gold mud is different from example 1 in that the gold mud is pretreated before the step (1), and the pretreatment is prepared by adopting a preparation example 1-1.
Example 4
A process for extracting gold from gold mud is different from example 3 in that pretreatment is carried out by adopting preparation examples 1-2.
Example 5
A process for extracting gold from gold mud is different from example 3 in that pretreatment is carried out by adopting preparation examples 1-3.
Example 6
A process for extracting gold from gold mud is different from example 3 in that pretreatment is carried out by adopting preparation examples 1-4.
Example 7
A process for extracting gold from gold mud is different from example 3 in that pretreatment is carried out by adopting preparation examples 1-5.
Example 8
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 6.
Example 9
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 7.
Example 10
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 8.
Example 11
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 9.
Example 12
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 10.
Example 13
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 11.
Example 14
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 12.
Example 15
The process for extracting gold from gold mud differs from example 1 in that the pretreatment was carried out using preparation examples 1 to 13.
Comparative example
Comparative example 1
The process for extracting gold from gold mud is different from example 1 in that the process comprises the following steps:
(1) Immersing 0.5kg of gold mud into a nitric acid solution with the mass concentration of 55%, reacting for 4 hours at the temperature of 55 ℃, filtering to perform solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 55min at the temperature of 70 ℃, then heating, reacting for 4h at the temperature of 100 ℃, wherein the mass ratio of the filter residue to the aqua regia is 1:7, filtering, performing solid-liquid separation, and collecting filtrate;
(3) Adding 0.8kg of reducing agent into the filtrate obtained in the step (2), reacting for 1h at 90 ℃ to obtain gold powder with the purity of 99.1%, washing, filtering, drying and smelting to obtain gold ingots.
Comparative example 2
The process for extracting gold from gold mud is different from example 1 in that the process comprises the following steps:
(1) Immersing 0.7kg of gold mud into a nitric acid solution with the mass concentration of 25%, reacting for 1h at the temperature of 75 ℃, filtering to perform solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 25min at the temperature of 85 ℃, then heating, reacting for 1h at the temperature of 90 ℃, wherein the mass ratio of the filter residue to the aqua regia is 1:1, filtering, performing solid-liquid separation, and collecting filtrate;
(3) Adding 0.2kg of reducing agent into the filtrate obtained in the step (2), reacting for 4 hours at the temperature of 75 ℃ to obtain gold powder with the purity of 99.0%, washing, filtering, drying and smelting to obtain gold ingots.
Performance test
The gold ingots obtained according to the processes of examples 1 to 15 and comparative examples 1 to 2 were tested, the content of impurity metals in the gold mud was analyzed, and the effect of removing impurity elements in the gold mud was calculated, and the results are shown in table 2.
The main metal element content of the gold mud adopted by the application is shown in table 1.
TABLE 1 analysis results of main elements of gold mud
| Element(s) | Au | Ag | Zn | Cu |
| Mass percent (%) | 19.56 | 70.12 | 0.048 | 0.013 |
| Element(s) | Ni | Fe | Pb | Al |
| Mass percent (%) | 0.56 | 3.45 | 2.15 | 0.018 |
Table 2 test data for examples and comparative examples
| Removal rate/% | Pb | Fe | Zn | Ni | Al | Cu |
| Example 1 | 89.93 | 89.95 | 89.90 | 89.25 | 89.63 | 89.72 |
| Example 2 | 89.91 | 89.91 | 89.87 | 89.12 | 89.65 | 89.70 |
| Example 3 | 99.92 | 99.94 | 99.91 | 99.24 | 99.62 | 99.71 |
| Example 4 | 96.56 | 96.55 | 96.45 | 96.12 | 96.15 | 96.32 |
| Example 5 | 96.75 | 96.74 | 96.68 | 96.31 | 96.45 | 96.42 |
| Example 6 | 99.91 | 99.94 | 99.89 | 99.23 | 99.62 | 99.70 |
| Example 7 | 96.82 | 96.91 | 96.89 | 96.79 | 96.78 | 96.86 |
| Example 8 | 99.91 | 99.92 | 99.88 | 99.21 | 99.61 | 99.70 |
| Example 9 | 92.12 | 92.15 | 91.00 | 91.68 | 91.79 | 91.98 |
| Example 10 | 96.89 | 96.78 | 96.65 | 96.45 | 96.25 | 96.40 |
| Example 11 | 96.91 | 96.79 | 96.72 | 96.47 | 96.28 | 96.42 |
| Example 12 | 99.91 | 99.92 | 99.87 | 99.22 | 99.61 | 99.70 |
| Example 13 | 96.99 | 96.89 | 96.78 | 96.89 | 96.56 | 96.78 |
| Example 14 | 99.91 | 99.90 | 99.90 | 99.20 | 99.61 | 99.70 |
| Example 15 | 99.90 | 99.91 | 99.89 | 99.21 | 99.20 | 99.69 |
| Comparative example 1 | 85.12 | 85.10 | 85.09 | 84.89 | 84.97 | 84.99 |
| Comparative example 2 | 85.10 | 85.08 | 85.08 | 84.87 | 84.95 | 84.97 |
Gold was extracted by the preparation method of example 3, and the purity of the finished gold ingot was measured by a gold ingot purity meter, and the result showed that the purity of gold was 99.8%.
As can be seen from Table 2, the impurity removal rate of the impurity Pb, fe, zn, ni, al, cu in the embodiment 1-2 of the application is about 89%, the gold mud is pretreated in the embodiment 3, the embodiment 6, the embodiment 8, the embodiment 12, the embodiment 14 and the embodiment 15, and the impurity removal rate of the impurity Pb, fe, zn, ni, al, cu is about 99%, which indicates that the grinding aid is used for pretreating the gold mud, so that the reaction efficiency of the gold mud and the nitric acid solution is improved, the copper, iron, zinc and other base metals and silver in the gold mud can be fast reacted with the nitric acid, and the extraction purity of gold is improved.
Example 4, in which no magnesium oxide was added during the pretreatment, showed that the magnesium oxide increased the grindability of the gold mud at about 96% for impurity Pb, fe, zn, ni, al, cu, and was effective to mix with the gold mud to facilitate the subsequent reaction of the gold mud with the nitric acid solution.
In the embodiment 5, no organic silicon is added in the pretreatment process, and the impurity removal rate of the impurity Pb, fe, zn, ni, al, cu is about 96%, which shows that the organic silicon can coat the surfaces of the fly ash particles, so that the oxidation resistance, the wear resistance and the corrosion resistance of the fly ash are further improved.
Example 7 changes the mass ratio of magnesia, fly ash and organosilicon, and as seen from table 2, the impurity removal rate for impurity Pb, fe, zn, ni, al, cu is higher than examples 4-5, but lower than examples 3 and 6, indicating that magnesia, fly ash and organosilicon have a synergistic effect, and magnesia is loaded on the surface and in the pores of fly ash, and organosilicon coats the fly ash, increasing the connectivity between fly ash and magnesia, further enhancing the corresponding properties of fly ash, and subsequently improving the dispersibility of the gold mud particles.
The fly ash of example 9 was not pretreated, and the impurity removal rate for impurity Pb, fe, zn, ni, al, cu was about 92%, which indicates that pretreatment of the fly ash improved the surface activity of the fly ash, enhanced the adsorptivity of the fly ash, and subsequently facilitated mixing of the fly ash with other components.
In the embodiment 10, no silane coupling agent is added in the fly ash pretreatment process, and the impurity removal rate of the impurity Pb, fe, zn, ni, al, cu is about 96%, which shows that the silane coupling agent carries out graft modification on the surface of the fly ash, so that the silane coupling agent and the fly ash carry out hydroxylation reaction, and the surface activity of the fly ash is improved.
In the embodiment 11, no chitosan is added in the fly ash pretreatment process, and the impurity removal rate of the impurity Pb, fe, zn, ni, al, cu is about 96%, so that the chitosan can coat the fly ash, the surface activity of the fly ash is further improved, the adsorptivity of the fly ash is enhanced, and the fly ash is subsequently mixed with other components.
Example 13 changes the mass ratio of fly ash, silane coupling agent and chitosan, and from table 2, the impurity removal rate for impurity Pb, fe, zn, ni, al, cu is higher than that of examples 10-11, but lower than that of examples 3 and 12, which shows that the fly ash, silane coupling agent and chitosan have synergistic effect, the silane coupling agent and the fly ash undergo crosslinking modification, and the chitosan and the silane coupling agent undergo grafting, so that the performance between the fly ash is improved, and the subsequent improvement of the corresponding performance of the fly ash as a grinding aid is facilitated.
Comparative examples 1-2 the reaction parameters in the process for extracting gold from gold mud were changed, and it is shown from table 2 that compared with example 1, the impurity removal rate for impurity Pb, fe, zn, ni, al, cu was about 85%, which indicates that each raw material component and the reaction parameters were proportioned according to a certain content so that gold mud had a higher purification rate, and the change of each raw material dosage and the change of the reaction conditions all affected the impurity removal rate for gold mud extraction.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The technological method for extracting gold from gold mud is characterized by comprising the following steps:
(1) Immersing gold mud into a nitric acid solution with the mass concentration of 35-45%, reacting for 2-3 hours at the temperature of 65-70 ℃, filtering for solid-liquid separation, and collecting filter residues;
(2) Immersing the filter residue obtained in the step (1) into aqua regia, reacting for 30-45min at the temperature of 75-80 ℃, then heating, reacting for 2-3h at the temperature of 95-98 ℃, filtering to perform solid-liquid separation, and collecting filtrate, wherein the mass ratio of the filter residue to the aqua regia is 1:2-5;
(3) Adding a reducing agent into the filtrate obtained in the step (2), reacting for 2-3 hours at the temperature of 80-85 ℃ to obtain gold powder with the purity of more than 99.5%, washing, filtering, drying and smelting to obtain gold ingots.
2. The process for extracting gold from gold mud according to claim 1, wherein the mass ratio of the gold mud to the nitric acid solution is 1:6-8.
3. The process for extracting gold from gold mud according to claim 1, wherein the reducing agent is one or more of sodium sulfite, oxalic acid and hydrazine hydrate.
4. The process for extracting gold from gold mud according to claim 1, wherein the gold mud is pretreated before the step (1), and the pretreatment comprises the following steps: dispersing gold mud in deionized water, adding a grinding aid, grinding, filtering, and drying to obtain pretreated gold mud; grinding aids include magnesium oxide, fly ash and silicones.
5. The process for extracting gold from gold mud according to claim 4, wherein the mass ratio of the magnesium oxide to the fly ash to the organic silicon is 0.1-0.3:1:0.06-0.08.
6. The process method for extracting gold from gold mud according to claim 4, wherein the mass ratio of the gold mud to the grinding aid is 1:0.3-0.6.
7. The process for extracting gold from gold mud according to claim 4, wherein the fly ash is pretreated by: pulverizing and sieving the fly ash to obtain fly ash fine powder, soaking the fly ash fine powder in a sulfuric acid solution with the mass fraction of 15% for 1-3h, washing the fly ash fine powder with water, adding the fly ash fine powder into a silane coupling agent, stirring the fly ash fine powder for 1-3h at 80-90 ℃, adding chitosan, continuously stirring the chitosan, washing the fly ash fine powder with water, filtering and drying the fly ash fine powder to obtain the modified fly ash.
8. The process for extracting gold from gold mud according to claim 7, wherein the mass ratio of the fly ash to the silane coupling agent to the chitosan is 1:2-5:0.06-0.09.
9. The process for extracting gold from gold mud according to claim 7, wherein the mass ratio of the fly ash to the sulfuric acid solution is 1:3-6.
10. The process for extracting gold from gold mud according to claim 7, wherein the stirring speed is 300-500r/min.
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