CN105441689A - Method for preparing high-purity gold - Google Patents
Method for preparing high-purity gold Download PDFInfo
- Publication number
- CN105441689A CN105441689A CN201510797300.1A CN201510797300A CN105441689A CN 105441689 A CN105441689 A CN 105441689A CN 201510797300 A CN201510797300 A CN 201510797300A CN 105441689 A CN105441689 A CN 105441689A
- Authority
- CN
- China
- Prior art keywords
- gold
- organic phase
- extraction
- bronze
- washing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting and preparing high-purity gold from a silver anode slime chlorination leaching solution. According to the method, the silver anode slime chlorination leaching solution is subjected to DBC two-stage extraction, impurity washing through hydrochloric acid, reverse extraction reduction through a sodium hydrogen sulfite solution and reduced gold powder boiling and drying, and gold powder which meets the national standard GB/T4134-2003 (2004-5-1) by 99.99% is prepared. In the process, the reduction rate of the gold powder is larger than 98%, and the international advanced level is reached. Rough gold powder produced through reverse extraction reduction is boiled and washed by pure water, and the times of boiling and washing are reduced to 1-3 from current 5-6; the consumption of chemical reagents is greatly reduced, emission of waste gas and waste water is reduced, the operation environment of workers is improved, and the labor intensity is lowered. According to the method, operation is convenient, linking of all processes is reasonable, the production period is short, the cost is low, and the operation environment is good. The method can be widely applied to extracting and preparing of gold from various anode slime chlorination leaching solutions.
Description
Technical field
The present invention relates to precious metal separation purification techniques, be specifically related to a kind of from silver anode slime chloridizing leach solution extraction prepare the method for High Purity Gold.
Background technology
The raw material that chlorination refining method gold refining technique adopts is mainly the anode sludge that silver-colored electrolysis produces, wherein the grade of silver is about 40%, in chloridizing leach solution solid-liquid separation process, filter worn by a small amount of silver chloride, and partial oxidation silver enters solution with the dissolving of the form of title complex, therefore, golden reduction process has part silver and is reduced, and causes argentiferous in bronze and cannot reach the quality standard that purity is 99.99%.
In addition, due to the complexity day by day of anode sludge raw material, element Pd is easy to enter in silver anode slime, and the reduction potential of palladium is near with metallographic, in gold reduction process, Pd is easy to be reduced out, thus cause a reduction ratio of gold lower, be only 80 ~ 85%, also there is larger gap with more than 90% index of international most advanced level; And in refining process, boil wash often to once reducing bronze nitric acid, the ammoniacal liquor produced, cause the waste gas that produces and wastewater flow rate large, cause that reagent consumption is large, worker's operating environment is severe.
Summary of the invention
The object of the invention is the deficiency in order to overcome above technology, providing the extraction from silver anode slime chloridizing leach solution that a kind of technical process is simple, yield is high, production cost is low to prepare the method for High Purity Gold.
The present invention prepares the method for High Purity Gold, utilize DBC(dibutyl carbitol) to silver anode slime chloridizing leach solution, two-stage extraction is carried out to the good extractibility of gold, obtain two-stage Gold-loaded organic phase, utilize the hydrochloric acid of 0.5 ~ 1mol/L to wash after being merged, remove impurity further; Recycling sodium sulfite solution carries out back extraction reduction to the Gold-loaded organic phase after pickling, filtration obtains thick bronze; Finally by thick bronze washing, oven dry, output more than 99.99% meets the qualified bronze of standard GB/T/T4134-2003 (2004-5-1).
Table 1 ingot GB/T4134-2003 (2004-5-1) chemical composition (%)
The composition (g/L) of above-mentioned silver anode slime chloridizing leach solution is: Au80.66, Ag0.058, Pt0.062, Pd0.31, Fe0.10, Pb0.0057, Sb0.00036, Bi0.00058, H
+3.05.
In the one-level extraction of two-stage extraction, the volume ratio of DBC and silver anode slime chloridizing leach solution is 2:1 ~ 3:1, leaves standstill, is separated, obtain Gold-loaded organic phase and one-level raffinate;
In secondary extraction, the volume ratio of DBC and one-level raffinate is 2:1 ~ 3:1, leaves standstill, is separated, obtain Gold-loaded organic phase and secondary raffinate.
During washing Gold-loaded organic phase, the volume ratio of hydrochloric acid and Gold-loaded organic phase is 1:1, washing time 5 ~ 15min.
The concentration of back extraction gold sodium sulfite solution used is 40%, and consumption is 1.2 ~ 1.5 times of theoretical amount, reaction churning time 30 ~ 45min, temperature 70 ~ 75 DEG C.
Thick bronze 95% washing with alcohol that back extraction goes out, to remove organic solvent residual on bronze; Then 100 DEG C of pure water 1 ~ 3 time is used, each 15 ~ 30min, to remove the impurity such as silver, palladium, hydrochloric acid be mixed with in bronze.
The present invention compared with prior art, has following beneficial effect:
The raw material that in the present invention, golden extraction process adopts is silver anode slime chloridizing leach solution, DBC is carried out two-stage extraction as extraction agent, adopt sodium sulfite solution as reductive agent back extraction gold after the Gold-loaded organic phase salt acid elution impurity obtained, the thick bronze obtained is through 95% washing with alcohol, poach, drying, obtain the qualified bronze that more than 99.99% meets standard GB/T/T4134-2003 (2004-5-1), the reduction ratio > 98% of bronze, reaches international most advanced level in the process; Adopt pure water to boil to the thick bronze of back extraction reduction generation to wash, and boil and wash number of times and be reduced to 1 ~ 3 time by 5 ~ 6 times of the prior art, save the consumption of chemical reagent dramatically, decrease the quantity discharged of waste gas and waste water, improve the operating environment of worker, reduce labour intensity.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
Below in conjunction with the drawings and specific embodiments, invention is described further.
Embodiment 1
Step 1: with pear shape separatory funnel, 100mLDBC and 50mL silver anode slime chloridizing leach solution is fully mixed 5min and carries out one-level extraction, is separated after leaving standstill 5min, obtains Gold-loaded organic phase 99.6mL and one-level raffinate 49.7mL;
Step 2: 100mLDBC is fully mixed 5min with above-mentioned one-level raffinate and carries out secondary extraction, is separated after leaving standstill 5min, obtains load organic phases 99.1mL and secondary raffinate 49.2mL, and secondary raffinate is used for displacement;
Step 3: two-stage is extracted the Gold-loaded organic phase obtained and merge, be the salt acid elution 5min of 0.5mol/L by 198.7mL concentration, leave standstill, isolate Gold-loaded organic phase 198.3mL after clarification;
Step 4: the Gold-loaded organic phase after above-mentioned pickling is placed in beaker is the sodium sulfite solution back extraction gold of 40% by 21mL concentration, reaction churning time 30min, temperature 70 C;
Step 5: filter, is separated and obtains organic phase after thick bronze and back extraction, 95% washing with alcohol of thick bronze 100mL 1 time;
Step 6: by the 100 DEG C of pure water 3 times of the thick bronze after 95% washing with alcohol, boil the time of washing is 15min at every turn, then dry and obtain the qualified bronze of 7.4406g, its composition (%) is: Ag0.0010, Cu0.00019, Fe0.00064, Bi0.00032, Sb0.00022, Pd0.00061, Pb0.00040, Cr0.00014, Sn0.00030, Mg0.00070, Mn0.00016, Ni0.00015, Si0.00011, As0.00067, and bronze reduction ratio is 98.1%.
Embodiment 2:
Step 1: with pear shape separatory funnel, 150mLDBC and 50mL silver anode slime chloridizing leach solution is fully mixed 5min and carries out one-level extraction, is separated after leaving standstill 5min, obtains Gold-loaded organic phase 149.5mL and one-level raffinate 49.7mL;
Step 2: 150mLDBC is fully mixed 5min with above-mentioned one-level raffinate and carries out secondary extraction, is separated after leaving standstill 5min, obtains Gold-loaded organic phase 149.7mL and secondary raffinate 49.5mL, and secondary raffinate is used for displacement;
Step 3: two-stage is extracted the Gold-loaded organic phase obtained and merge, be the salt acid elution 5min of 0.5mol/L by 299.2mL concentration, leave standstill, isolate Gold-loaded organic phase 299.0mL after clarification;
Step 4: the Gold-loaded organic phase after above-mentioned pickling is placed in beaker is 40% sodium sulfite solution back extraction gold by 26mL concentration, reaction churning time 35min, temperature 75 DEG C;
Step 5: filter, is separated and obtains organic phase after thick bronze and back extraction, 95% washing with alcohol of thick bronze 100mL 1 time;
Step 6: by the 100 DEG C of pure water 2 times of the thick bronze after 95% washing with alcohol, boil the time of washing is 20min at every turn, then dry and obtain qualified bronze 8.548g, its composition (%) is: Ag0.0010, Cu0.00019, Fe0.00064, Bi0.00032, Sb0.00022, Pd0.00061, Pb0.00040, Cr0.00014, Sn0.00010, Mg0.00010, Mn0.00016, Ni0.00010, Si0.00011, As0.00047, and bronze reduction ratio is 98.15%.
Embodiment 3:
Step 1: in 5L beaker, 2LDBC and 1L silver anode slime chloridizing leach solution is stirred 10min makes it fully mix, and carries out one-level extraction, by most of organic phase and aqueous phase separation after standing 10min, not segregative separating funnel is separated, and obtains 1.8L Gold-loaded organic phase and 0.9L one-level raffinate;
Step 2: 2LDBC is stirred 10min with above-mentioned one-level raffinate and makes it fully mix, carry out secondary extraction, is separated after leaving standstill 10min, obtains 1.7L Gold-loaded organic phase and 0.8L secondary raffinate, and secondary raffinate is used for displacement;
Step 3: two-stage is extracted the Gold-loaded organic phase obtained and merge, be the salt acid elution of 1mol/L by 3.5L concentration in 10L glass reaction still, and reaction churning time 10min, leaves standstill 15min, isolate Gold-loaded organic phase 3.4L after clarification;
Step 4: the Gold-loaded organic phase after above-mentioned pickling is placed in 10L glass reaction still is the sodium sulfite solution back extraction gold of 40% by 160mL concentration, reaction churning time 40min, temperature 70 C;
Step 5: filter, is separated and obtains organic phase after thick bronze and back extraction, 95% washing with alcohol of thick bronze 1000mL 2 times;
Step 6: by the 100 DEG C of pure water 2 times of the thick bronze after 95% washing with alcohol, boil the time of washing is 25min at every turn, then dry and obtain qualified bronze 89.7988g, its composition (%) is: Ag0.00010, Cu0.00010, Fe0.00064, Bi0.00032, Sb0.00022, Pd0.00061, Pb0.00040, Cr0.00014, Sn0.00010, Mg0.00010, Mn0.00016, Ni0.00010, Si0.00011, As0.00030, and bronze reduction ratio is 99.2%.
Embodiment 4:
Step 1: in 5L beaker, 2LDBC and 1L silver anode slime chloridizing leach solution is stirred 15min makes it fully mix, and carries out one-level extraction, by most of organic phase and aqueous phase separation after standing 15min, not segregative separating funnel is separated, and obtains 1.9L Gold-loaded organic phase and 0.9L one-level raffinate;
Step 2: 2LDBC is stirred 15min with above-mentioned one-level raffinate and makes it fully mix, carry out secondary extraction, be separated after leaving standstill 15min and obtain 1.8L Gold-loaded organic phase and 0.8L secondary raffinate, secondary raffinate is used for displacement;
Step 3: two-stage is extracted the Gold-loaded organic phase obtained and merge, be the salt acid elution of 1mol/L by 3.7L concentration in 10L glass reaction still, and reaction churning time 15min, leaves standstill 15min, isolate 3.6L Gold-loaded organic phase after clarification;
Step 4: the Gold-loaded organic phase after above-mentioned pickling is placed in 10L glass reaction still is the sodium sulfite solution back extraction gold of 40% by 162mL concentration, reaction churning time 45min, temperature 75 DEG C;
Step 5: filter, is separated and obtains organic phase after thick bronze and back extraction, 95% washing with alcohol of thick bronze 1000mL 1 time;
Step 6: by the 100 DEG C of pure water 1 time of the thick bronze after 95% washing with alcohol, boil the time of washing is 30min at every turn, then dry and obtain the qualified bronze of 90.6652g, its composition (%) is: Ag0.00079, Cu0.0001, Fe0.00064, Bi0.00032, Sb0.00010, Pd0.00022, Pb0.00020, Cr0.00014, Sn0.00010, Mg0.00010, Mn0.00016, Ni0.00010, Si0.00011, As0.00033, and bronze reduction ratio is 99.37%.
Claims (2)
1. prepare a method for High Purity Gold, it is characterized in that being undertaken by following processing step:
(1) DBC and silver anode slime chloridizing leach solution are fully mixed with volume ratio 2:1 ~ 3:1 carry out one-level extraction, leave standstill, be separated after clarification, obtain Gold-loaded organic phase and one-level raffinate;
(2) DBC and one-level raffinate are mixed with volume ratio 2:1 ~ 3:1 carry out secondary extraction, leave standstill, be separated after clarification, obtain Gold-loaded organic phase and secondary raffinate;
(3) two-stage is extracted the Gold-loaded organic phase obtained to merge, wash 5 ~ 15min with the hydrochloric acid of 0.5 ~ 1mol/L with volume ratio 1:1;
(4) with the gold in Gold-loaded organic phase after the above-mentioned pickling of 40% sodium sulfite solution back extraction, sodium sulfite solution consumption is 1.2 ~ 1.5 times of theoretical amount, reaction churning time 30 ~ 45min, temperature 70 ~ 75 DEG C;
(5) filter, be separated and obtain organic phase after thick bronze and back extraction, thick bronze 95% washing with alcohol;
(6) by the 100 DEG C of pure water 1 ~ 3 time of the thick bronze after 95% washing with alcohol, each 15 ~ 30min, obtains qualified bronze after oven dry.
2. a kind of method preparing High Purity Gold according to claim 1, is characterized in that: the composition (g/L) of described silver anode slime chloridizing leach solution is: Au80.66, Ag0.058, Pt0.062, Pd0.31, Fe0.10, Pb0.0057, Sb0.00036, Bi0.00058, H
+3.05.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510797300.1A CN105441689A (en) | 2015-11-18 | 2015-11-18 | Method for preparing high-purity gold |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510797300.1A CN105441689A (en) | 2015-11-18 | 2015-11-18 | Method for preparing high-purity gold |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105441689A true CN105441689A (en) | 2016-03-30 |
Family
ID=55552311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510797300.1A Pending CN105441689A (en) | 2015-11-18 | 2015-11-18 | Method for preparing high-purity gold |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105441689A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363920A (en) * | 2020-04-07 | 2020-07-03 | 金川集团股份有限公司 | Method for extracting gold from silver-containing liquid |
| CN114769580A (en) * | 2022-03-09 | 2022-07-22 | 金川集团股份有限公司 | Method for removing impurity silver from reduced gold powder |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
| US20120234138A1 (en) * | 2011-03-18 | 2012-09-20 | Jx Nippon Mining & Metals Corporation | Method of recovering gold from dilute gold solution |
| CN103074492A (en) * | 2013-01-24 | 2013-05-01 | 贵研资源（易门）有限公司 | Method for separating and purifying gold from noble metal solution |
| WO2014062289A1 (en) * | 2012-10-19 | 2014-04-24 | Kennecott Utah Copper Llc | Process for the recovery of gold form anode slimes |
| CN103757246A (en) * | 2014-01-02 | 2014-04-30 | 紫金矿业集团股份有限公司 | Method for producing high-purity gold |
| CN104480322A (en) * | 2014-12-07 | 2015-04-01 | 金川集团股份有限公司 | Method for extracting gold and palladium from silver anode slime |
| JP2015105413A (en) * | 2013-11-29 | 2015-06-08 | 住友金属鉱山株式会社 | Method for manufacturing gold powder with high bulk density |
-
2015
- 2015-11-18 CN CN201510797300.1A patent/CN105441689A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
| US20120234138A1 (en) * | 2011-03-18 | 2012-09-20 | Jx Nippon Mining & Metals Corporation | Method of recovering gold from dilute gold solution |
| WO2014062289A1 (en) * | 2012-10-19 | 2014-04-24 | Kennecott Utah Copper Llc | Process for the recovery of gold form anode slimes |
| CN103074492A (en) * | 2013-01-24 | 2013-05-01 | 贵研资源（易门）有限公司 | Method for separating and purifying gold from noble metal solution |
| JP2015105413A (en) * | 2013-11-29 | 2015-06-08 | 住友金属鉱山株式会社 | Method for manufacturing gold powder with high bulk density |
| CN103757246A (en) * | 2014-01-02 | 2014-04-30 | 紫金矿业集团股份有限公司 | Method for producing high-purity gold |
| CN104480322A (en) * | 2014-12-07 | 2015-04-01 | 金川集团股份有限公司 | Method for extracting gold and palladium from silver anode slime |
Non-Patent Citations (3)
| Title |
|---|
| 朱建良等: "从铅阳极泥中回收有价金属新工艺", 《南京工业大学学报(自然科学版)》 * |
| 长沙矿冶研究院等: "二丁基卡必醇萃取法提金扩大试验和试生产的工艺研究", 《矿冶工程》 * |
| 长沙矿冶研究院等: "二丁基卡必醇萃取法提金的研究", 《矿冶工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363920A (en) * | 2020-04-07 | 2020-07-03 | 金川集团股份有限公司 | Method for extracting gold from silver-containing liquid |
| CN114769580A (en) * | 2022-03-09 | 2022-07-22 | 金川集团股份有限公司 | Method for removing impurity silver from reduced gold powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106119554B (en) | High Purity Gold and the method for being enriched with silver, platinum and palladium are prepared from silver anode slime | |
| CN101565174B (en) | Method for extracting refined tellurium from tellurium-contained smelting slag | |
| CN107460324B (en) | A kind of method that silver anode slime control current potential prepares four or nine gold medals | |
| CN102994771B (en) | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid | |
| CN105132693B (en) | The technique of Recover palladium in a kind of sour palladium waste liquid after activation from colloidal activating palladium | |
| CN103374659B (en) | Valuable, the refinement recovery method of rare metal in a kind of garbage | |
| CN100342044C (en) | Technological process for extracting gold, silver and palladium from electronic industry waste | |
| CN111575483B (en) | Method for separating selenium, tellurium, arsenic, copper, lead and silver and enriching gold from copper anode slime | |
| CN105274351B (en) | The technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole | |
| CN103045849B (en) | Pretreatment method for platinum palladium concentrate | |
| CN106636652A (en) | Technique for efficient and environment-friendly recovery of palladium from sliver anode slime parting liquid | |
| CN103509953A (en) | Method for pre-treating high-impurity copper anode slime rich in noble metals | |
| CN106086417A (en) | A kind of method extracting copper and gold from waste mobile phone circuit board | |
| CN109231175A (en) | A method of impure selenium is purified with dehydrated alcohol | |
| CN113308606A (en) | Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag | |
| CN105965030A (en) | Technique for recovering gold from gold iodide liquid waste | |
| CN104876260A (en) | Method for preparing tin dioxide directly by using tin-electrolyzed anode mud | |
| CN105886785A (en) | Method for preparing high-purity silver powder from silver-rich residue containing high selenium and tellurium | |
| CN112210674A (en) | Production process of high-purity gold | |
| CN105441689A (en) | Method for preparing high-purity gold | |
| CN106834691A (en) | A kind of copper anode mud wet-treating comprehensive recycling process | |
| CN116716484B (en) | Method for recovering palladium and dimethylglyoxime from palladium-refining palladium-removing slag | |
| CN109402402B (en) | Method for recovering gold and silver from gold-silver-copper alloy waste | |
| CN103834811A (en) | Method for selectively extracting gold from complex gold-containing waste | |
| CN106756047B (en) | High sundries silver anode slime puies forward the processing method of gold |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160330 |
|
| RJ01 | Rejection of invention patent application after publication |