CN108220615B - Gold purification process - Google Patents
Gold purification process Download PDFInfo
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- CN108220615B CN108220615B CN201810021011.6A CN201810021011A CN108220615B CN 108220615 B CN108220615 B CN 108220615B CN 201810021011 A CN201810021011 A CN 201810021011A CN 108220615 B CN108220615 B CN 108220615B
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- 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
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- 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
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention relates to the technical field of precious metal purification, in particular to a gold purification process, which comprises the steps of raw material pretreatment, mixed reagent treatment, gold leaching, enrichment and separation. By utilizing the purification process, on one hand, the removal rate of base metals and other precious metals can be improved, and the purity of gold is greatly improved; on the other hand, the dissolution of gold is promoted, and the extraction rate of gold is improved.
Description
Technical Field
The invention relates to the technical field of precious metal purification, in particular to a gold purification process.
Background
At present, there are many technological methods for extracting gold from ores at home and abroad, such as electrolytic methods, chemical methods, ion exchange methods and extraction methods. Although the extraction processes can extract gold from the ores to a certain extent, the purity of the gold is not high, and a large amount of gold elements in the ores are wasted in the extraction process, so that the extraction rate of the gold is not high, the waste is large, and the gold resource loss is caused; therefore, in order to solve the above problems, it is necessary to establish a new purification process.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the prior art, the gold purification process is provided, the purity of gold can be greatly improved by utilizing the purification process, and the extraction rate of gold is also improved.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a process for the purification of gold, said purification process comprising the steps of:
(1) pretreatment of raw materials: crushing and screening gold ore, adding sulfuric acid into the obtained gold ore powder, mixing, heating, stirring, adding an oxidant, filtering after the reaction is finished, and respectively collecting leachate and gold-containing filter residue;
(2) mixed medicament treatment: adding sodium lignosulphonate into the gold-containing filter residue obtained in the step (1), adding the mixed medicament, heating, stirring, filtering after the reaction is finished, and respectively collecting leachate and the gold-containing filter residue;
(3) gold leaching: adding a mixture of chloride and hypochlorite into the gold-containing filter residue obtained in the step (2), stirring, adding an oxidant, heating, pressurizing, and reacting for a period of time to obtain slurry;
(4) enrichment: taking the slurry in the step (3), adding extraction resin, stirring, heating, treating for a period of time, filtering, and respectively collecting leachate and solid filtrate;
(5) separation: and (4) adding a desorbent into the solid filtrate obtained in the step (4), heating, stirring, adding a reducing agent, heating, stirring, filtering and collecting crude gold powder, and carrying out acid washing, hot water washing and drying on the crude gold powder to obtain a finished product.
As an improved technical scheme, the concentration of the sulfuric acid in the step (1) is 45-60 wt%, and the sulfuric acid and the gold ore powder are added according to the liquid-solid ratio of 5-10: 1.
As an improved technical scheme, the oxidant in the step (1) is sodium peroxide or hydrogen peroxide.
As a preferable technical scheme, the mixed medicament in the step (2) comprises 75-85 wt% of concentrated sulfuric acid and a mixture of perchloric acid and NK8310 chelating resin, and the mixture of the perchloric acid and the NK8310 chelating resin is mixed according to the mass ratio of 3.5-4: 0.15-3.
As an improved technical scheme, the adding amount of the sodium lignosulphonate in the step (2) is 0.1-0.5% of the weight of the gold-containing filter residue.
As an improved technical scheme, the chloride in the step (3) is sodium chloride or potassium chloride; the hypochlorite is sodium hypochlorite, potassium hypochlorite or calcium hypochlorite; the oxidant is manganese dioxide.
As an improved technical scheme, the extraction resin in the step (4) is PS0+ P350 resin, N503 resin or bisphenol A type poly-crown ether resin, and the addition amount of the extraction resin is 1.5-3 times of the weight of the slurry.
As an improved technical scheme, the desorbent in the step (5) is a thiourea solution and a mixed solution of the thiourea solution and hydrochloric acid, and the addition amount of the desorbent is 0.3-1 time of the weight of the extraction resin.
As an improved technical scheme, the reducing agent in the step (5) is trisodium citrate or white phosphorus, and the addition amount of the reducing agent is 0.2-0.8 times of the weight of the desorbent.
As a preferable technical scheme, the temperature of the heating in the step (1) and the step (2) is controlled to be 95-100 ℃, and the temperature of the heating in the step (3) is controlled to be 45-65 ℃.
After the technical scheme is adopted, the invention has the beneficial effects that:
(1) the method adopts sulfuric acid and oxidant for heating treatment, metal copper, iron, zinc, lead, nickel and silver in the gold raw material respectively react with the sulfuric acid to be converted into ions to enter the solution, and part of impurity metal can be effectively removed through filtering; sodium lignosulfonate and mixed agents (sulfuric acid, perchloric acid and NK8310 chelating resin) are added for treatment, and the addition of the sodium lignosulfonate can reduce the wrapping or agglomeration of sulfide on gold and is more favorable for leaching the gold; when the mixed reagent is treated, sulfuric acid is added firstly, silver and other base metals remained in gold ore powder react with the sulfuric acid firstly to form silver sulfate slightly-soluble substances and base metal ions, perchloric acid and NK8310 chelating resin are added, the silver sulfate can be dissolved by the perchloric acid, and then the silver ions and the base metal ions are adsorbed by polyester thiourea resin, so that the effective separation of the silver and the remained lead, copper and gold is realized, and the consumption of hypochlorite in a gold leaching link is reduced; through the treatment of the three processes, the removal rate of base metals and other noble metals is over 99.99 percent;
(2) according to the invention, the gold is leached by chloride and hypochlorite, the reaction temperature and pressure are controlled under the action of manganese dioxide, and the gold element in the gold ore powder fully reacts with sodium/potassium chloride and hypochlorite to form a large amount of gold-chlorine complexes; adsorbing the gold-loaded slurry by using the extraction resin, filtering and collecting filter residues, performing the action of a desorbent on the filter residues, completely releasing gold enriched by the extraction resin, and converting the gold enriched by the extraction resin into gold powder under the action of a reducing agent;
(3) the process method of the invention has simple operation, stable and reliable product quality, the purity of the gold can reach more than 99.999 percent, and the extraction rate of the gold is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A process for purifying gold, comprising the steps of:
(1) pretreatment of raw materials: crushing and screening gold ore, adding 45 wt% sulfuric acid into the obtained gold ore powder according to the solid-to-liquid ratio of 1:5, mixing, heating to 95 ℃, stirring, adding an oxidant (sodium peroxide or hydrogen peroxide) accounting for 0.5% of the weight of the gold ore powder, filtering after the reaction is finished, and respectively collecting leachate and gold-containing filter residue;
(2) mixed medicament treatment: adding sodium lignosulfonate accounting for 0.15% of the weight of the gold-containing filter residue in the step 1 into the gold-containing filter residue, stirring, adding a mixed medicament (the molar ratio of a mixture of sulfuric acid to perchloric acid to NK8310 chelating resin is 0.5:1, the molar ratio of the mixture of perchloric acid to NK8310 chelating resin is calculated by perchloric acid, and the mixture of perchloric acid and NK8310 chelating resin is mixed according to the mass ratio of 3.5: 0.17) according to the solid-to-liquid ratio of 1: 2.5), stirring, heating to 95 ℃, filtering after the reaction is finished, and respectively collecting leachate and the gold-containing filter residue;
(3) gold leaching: taking the gold-containing filter residue in the step (2), adding a mixture of chloride and hypochlorite according to a solid-to-liquid ratio of 1:2.5 (the chloride and the hypochlorite are composed according to a molar ratio of 0.2: 0.15), stirring, adding manganese dioxide accounting for 0.2% of the weight of the gold-containing filter residue, heating to 45 ℃, pressurizing, and reacting for a period of time to obtain slurry;
(4) enrichment: taking the slurry in the step (3), adding extraction resin (PS0+ P350 resin) which is 1.5 times of the weight of the slurry, stirring, heating, treating for a period of time, filtering, and respectively collecting leachate and filter residue;
(5) separation: and (3) adding a desorbent (0.15mol/l thiourea solution) which is 0.3 time of the weight of the extraction resin into the filter residue obtained in the step (4), heating, stirring, adding a reducing agent (trisodium citrate) which is 0.2 time of the weight of the desorbent, reheating, stirring, filtering and collecting the crude gold powder, and carrying out acid washing, hot water washing and drying on the crude gold powder to obtain a finished product.
Under the condition of the process, the removal rate of base metals and other noble metals is 99.994%, and the purity of gold is more than 99.999%.
Example 2
A process for purifying gold, comprising the steps of:
(1) pretreatment of raw materials: crushing and screening gold ore, adding 55 wt% sulfuric acid into the obtained gold ore powder according to the solid-to-liquid ratio of 1:8, mixing, heating to 98 ℃, stirring, adding an oxidant (sodium peroxide or hydrogen peroxide) accounting for 0.8% of the weight of the gold ore powder, filtering after the reaction is finished, and respectively collecting leachate and gold-containing filter residue;
(2) mixed medicament treatment: adding sodium lignosulfonate accounting for 0.4 percent of the weight of the gold-containing filter residue in the step 1 into the gold-containing filter residue, adding a mixed medicament (the molar ratio of a mixture of sulfuric acid to perchloric acid to NK8310 chelating resin is 1.5:2, the molar ratio of the mixture of the perchloric acid to the NK8310 chelating resin is calculated by the perchloric acid, and the mixture of the perchloric acid and the NK8310 chelating resin is mixed according to the mass ratio of 3.7: 2) according to a solid-to-liquid ratio of 1:6, heating to 98 ℃, stirring, filtering after the reaction is finished, and respectively collecting leachate and the gold-containing filter residue;
(3) gold leaching: taking the gold-containing filter residue in the step (2), adding a mixture of chloride and hypochlorite according to a solid-to-liquid ratio of 1:6 (the chloride and the hypochlorite are composed according to a molar ratio of 0.4: 0.3), stirring, adding manganese dioxide accounting for 0.45% of the weight of the gold-containing filter residue, heating to 62 ℃, pressurizing, and reacting for a period of time to obtain slurry;
(4) enrichment: taking the slurry in the step (3), adding extraction resin (bisphenol A type poly-crown ether resin) which is 2.5 times of the weight of the slurry, stirring, heating, treating for a period of time, filtering, and respectively collecting leachate and filter residue;
(5) separation: and (3) adding a desorbent (the volume ratio of thiourea solution with the concentration of 0.25mol/l to hydrochloric acid is 1: 0.5) which is 0.8 times of the weight of the extraction resin into the filter residue obtained in the step (4), heating, stirring, adding a reducing agent (trisodium citrate) which is 0.6 times of the weight of the desorbent, reheating, stirring, filtering and collecting crude gold powder, and carrying out acid washing, hot water washing and drying to obtain a finished product.
Under the condition of the process, the removal rate of base metals and other noble metals is 99.997%, and the purity of gold is more than 99.999%.
Example 3
A process for purifying gold, comprising the steps of:
(1) pretreatment of raw materials: crushing and screening gold ore, adding 60 wt% sulfuric acid into the obtained gold ore powder according to the solid-to-liquid ratio of 1:10, mixing, heating to 100 ℃, stirring, adding an oxidant (sodium peroxide or hydrogen peroxide) accounting for 1% of the weight of the gold ore powder, filtering after the reaction is finished, and respectively collecting leachate and gold-containing filter residue;
(2) mixed medicament treatment: taking the gold-containing filter residue obtained in the step 1, adding sodium lignosulfonate accounting for 0.5% of the weight of the gold-containing filter residue, adding a mixed medicament (the molar ratio of a mixture of sulfuric acid to perchloric acid to NK8310 chelating resin is 2:3, the molar ratio of the mixture of perchloric acid to NK8310 chelating resin is calculated by perchloric acid, and the mixture of perchloric acid and NK8310 chelating resin is mixed according to the mass ratio of 4: 3) according to the solid-to-liquid ratio of 1:8, heating to 100 ℃, stirring, filtering after the reaction is finished, and respectively collecting a leaching solution and the gold-containing filter residue;
(3) gold leaching: taking the gold-containing filter residue in the step (2), adding a mixture of chloride and hypochlorite according to a solid-to-liquid ratio of 1:8 (the chloride and the hypochlorite are in a molar ratio of 0.5: 0.48), stirring, adding manganese dioxide accounting for 0.5% of the weight of the gold-containing filter residue, heating to 65 ℃, pressurizing, and reacting for a period of time to obtain slurry;
(4) enrichment: taking the slurry in the step (3), adding extraction resin (N503 resin) which is 3 times of the weight of the slurry, stirring, heating, treating for a period of time, filtering, and respectively collecting leachate and filter residue;
(5) separation: and (3) taking the filter residue obtained in the step (4), adding a desorbent (0.28mol/l thiourea solution and hydrochloric acid are mixed according to the ratio of 1: 1) which is 1 time of the weight of the extraction resin, heating, stirring, adding a reducing agent (trisodium citrate) which is 0.8 time of the weight of the desorbent, reheating, stirring, filtering and collecting the crude gold powder, and carrying out acid washing, hot water washing and drying to obtain a finished product.
Under the condition of the process, the removal rate of base metals and other noble metals is 99.996%, and the purity of gold is more than 99.999%.
In order to better prove that the process method has better removal rate for base metals and other precious metals, short extraction phase separation time and high gold purity, the invention also provides 3 comparative examples.
Comparative example 1
Different from the example 2, the step (2) does not adopt the mixed medicament treatment, but adopts the nitric acid treatment with 60-80 wt%, and the rest conditions are the same, under the process conditions, the removal rate of base metals and other precious metals is 99.78%, and the purity of gold is less than 99.999%.
Comparative example 2
Different from the embodiment 2, the mixed medicament in the step (2) is not added with sodium lignosulfonate during the treatment, the other conditions are the same, the removal rate of the base metal and other noble metals under the process conditions is 99.85 percent, and the purity of the gold is less than 99.999 percent.
Comparative example 3
Different from the embodiment 2, no manganese dioxide is added during the gold leaching in the step (3), the other conditions are the same, the removal rate of base metals and other precious metals under the process conditions is 99.99%, and the purity of gold is less than 99.999%.
Claims (9)
1. A purification process of gold, characterized in that the purification process comprises the following steps:
(1) pretreatment of raw materials: crushing and screening gold ore, adding sulfuric acid into the obtained gold ore powder, mixing, heating, stirring, adding an oxidant, filtering after the reaction is finished, and respectively collecting leachate and gold-containing filter residue;
(2) mixed medicament treatment: adding the gold-containing filter residue obtained in the step (1) into sodium lignosulphonate, stirring,
adding the mixed medicament, heating, stirring, filtering after the reaction is finished, and respectively collecting the leaching solution and the gold-containing filter residue; the mixed medicament comprises 75-85 wt% of concentrated sulfuric acid and a mixture of perchloric acid and NK8310 chelating resin, wherein the mixture of perchloric acid and NK8310 chelating resin is mixed according to the mass ratio of 3.5-4: 0.15-3.
(3) Gold leaching: adding a mixture of chloride and hypochlorite into the gold-containing filter residue obtained in the step (2), stirring, adding an oxidant, heating, pressurizing, and reacting for a period of time to obtain slurry;
(4) enrichment: taking the slurry in the step (3), adding extraction resin, stirring, heating, treating for a period of time, filtering, and respectively collecting leachate and solid filtrate;
(5) separation: and (4) adding a desorbent into the solid filtrate obtained in the step (4), heating, stirring, adding a reducing agent, heating, stirring, filtering and collecting crude gold powder, and carrying out acid washing, hot water washing and drying on the crude gold powder to obtain a finished product.
2. The process of claim 1, wherein the gold is purified by: in the step (1), the concentration of the sulfuric acid is 45-60 wt%, and the sulfuric acid and the gold ore powder are added according to the liquid-solid ratio of 5-10: 1.
3. The process of claim 1, wherein the gold is purified by: the oxidant in the step (1) is sodium peroxide or hydrogen peroxide.
4. The process of claim 1, wherein the gold is purified by: the adding amount of the sodium lignosulphonate in the step (2) is 0.1-0.5% of the weight of the gold-containing filter residue.
5. The process of claim 1, wherein the gold is purified by: in the step (3), the chloride is sodium chloride or potassium chloride; the hypochlorite is sodium hypochlorite, potassium hypochlorite or calcium hypochlorite; the oxidant is manganese dioxide.
6. The process of claim 1, wherein the gold is purified by: and (4) the extraction resin in the step (4) is N503 resin, and the addition amount of the extraction resin is 1.5-3 times of the weight of the slurry.
7. The process of claim 1, wherein the gold is purified by: in the step (5), the desorbent is a thiourea solution, a mixed solution of the thiourea solution and hydrochloric acid, and the addition amount of the desorbent is 0.3-1 time of the weight of the extraction resin.
8. The process of claim 1, wherein the gold is purified by: in the step (5), the reducing agent is trisodium citrate or white phosphorus, and the addition amount of the reducing agent is 0.2-0.8 times of the weight of the desorbent.
9. The process of claim 1, wherein the gold is purified by: the temperature of the step (1) and the step (2) is controlled to be 95-100 ℃ during heating, and the temperature of the step (3) is controlled to be 45-65 ℃.
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| CN201810021011.6A CN108220615B (en) | 2018-01-10 | 2018-01-10 | Gold purification process |
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| CN109499625B (en) * | 2018-11-06 | 2021-09-28 | 长春黄金研究院有限公司 | High-efficiency elution method for gold-loaded resin |
| CN111321299B (en) * | 2020-03-23 | 2021-12-14 | 紫金矿业集团股份有限公司 | Method for efficiently separating silver, platinum and palladium from silver anode mud |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362532A (en) * | 2001-01-08 | 2002-08-07 | 冶金工业部长春黄金研究院 | Amminochloride process of purifying gold |
| CN101715493A (en) * | 2007-05-18 | 2010-05-26 | 塞瑟尔有限公司 | Process for precious metal recovery from a sulphide ore or concentrate or other feed material |
| CN104694764A (en) * | 2015-03-09 | 2015-06-10 | 中南大学 | Reinforced leaching method of fine-grained encapsulated gold |
| AU2013263848A1 (en) * | 2013-11-29 | 2015-06-18 | Lifezone Limited | Treatment process for extraction of metals from ores |
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- 2018-01-10 CN CN201810021011.6A patent/CN108220615B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362532A (en) * | 2001-01-08 | 2002-08-07 | 冶金工业部长春黄金研究院 | Amminochloride process of purifying gold |
| CN101715493A (en) * | 2007-05-18 | 2010-05-26 | 塞瑟尔有限公司 | Process for precious metal recovery from a sulphide ore or concentrate or other feed material |
| AU2013263848A1 (en) * | 2013-11-29 | 2015-06-18 | Lifezone Limited | Treatment process for extraction of metals from ores |
| CN104694764A (en) * | 2015-03-09 | 2015-06-10 | 中南大学 | Reinforced leaching method of fine-grained encapsulated gold |
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| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 262400 building 19, No. 1388, Baoshi City Second Road, Changle Economic Development Zone, Weifang City, Shandong Province Patentee after: ZHONGBAO ZHENGXIN GOLD AND SILVER JEWELRY DETECTION Co.,Ltd. Address before: 262400 building 16, Xincheng street, Changle County, Weifang, Shandong, 16 Patentee before: ZHONGBAO ZHENGXIN GOLD AND SILVER JEWELRY DETECTION Co.,Ltd. |