CN1442498A - Method of crude gold purification - Google Patents

Method of crude gold purification Download PDF

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Publication number
CN1442498A
CN1442498A CN 03112144 CN03112144A CN1442498A CN 1442498 A CN1442498 A CN 1442498A CN 03112144 CN03112144 CN 03112144 CN 03112144 A CN03112144 A CN 03112144A CN 1442498 A CN1442498 A CN 1442498A
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gold
solution
purified
thick gold
thick
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CN 03112144
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CN1208482C (en
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陈光辉
王德煜
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Shandong gold mining Limited by Share Ltd
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JIAOJIA GOLD MINE SHANDONG GOLD GROUP CO Ltd
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Abstract

A process for purifying raw gold whose purity is 85-99.5% includes such steps as electrolysis in which said raw gold is used to make anode plate, pure gold or titanium is used to make cathode, the ceramic crucible is used as the diaphragm of cathode and diluted hydrochloric acid is uses a electrolyte to conver the raw gold to gold solution, and reducing the gold solution to gold powder No.1. Its advantages are low requirement to raw gold and low cost.

Description

The method that a kind of thick gold is purified
(1) technical field
The present invention relates to a kind of grade less than 99.5% thick golden method of purification, belong to golden purification techniques field.
(2) background technology
At present, the domestic refining that generally adopts is cast positive plate with thick gold, utilizes the effect of electric current, and gold is dissolved on anode, selects to separate out on negative electrode and reaches the purpose of purification.Domestic manufacturer has between Great Wall, Chengdu refinery, Inner Mongol universe refinery, the comprehensive recovery vehicle of Shenyang Smeltery Factory etc.This kind method is quite ripe both at home and abroad, but this method have a following shortcoming: the one, the electrolysis gold grade will reach national 1# gold, the anode gold grade generally reaches more than 99.5%, that is to say that this method is suitable for handling grade at the thick gold more than 99.5%, just can carry out electrolysis after must pre-treatment reaching 99.5% for grade less than 99.5% thick gold; The 2nd, it is more that this kind method flow overstocks gold.
The external general efflorescence technology that adopts is made powder with thick gold, then with chloroazotic acid or chlorine leach, and last reductive purification techniques.Sweden Bo Lideng company is abroad arranged, and domestic have Central Plains, Henan gold smelting factory, a Zhaoyuan gold and silver refinery etc.This kind method can be handled the thick gold of various grades, but because domestic efflorescence equipment does not reach the fineness of requirement, and equipment can only rely on import, equipment importation approximately needs 3,000,000 yuan of Renminbi, invests bigger; The production run cost is higher in addition.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of and carry out the method that thick gold is purified with electrochemical solution, reduction purification techniques.
The technical scheme of the inventive method is as follows:
The thick gold of raw material is cast as Jinyang pole plate, and electrochemical solution makes gold be converted into gold solution, and control solution Gold Content or controlled oxidation reduction potential are reduced to gold solution with reductive agent the 1# bronze of national regulation.
The electrochemical solution of the inventive method is to make positive plate with thick gold, makes negative electrode with proof gold or titanium plate, carries out electrolysis with dilute hydrochloric acid as electrolytic solution, and electrolyzer is pottery or plastic channel, and negative electrode is made barrier film with the biscuit ware crucible.
Electrolytic solution dilute hydrochloric acid is HCl in the above-mentioned electrolyzer: H 2O=1.5~3: 1, electrolytic solution dilute hydrochloric acid is HCl in the crucible: H 2O=1~2: 1~2.
Liquid level is higher than electrolyzer liquid level 5~10mm in the above-mentioned crucible.
Feed pulsatory current, the thick gold dissolving of anode, gold is with Au 3+Enter in the anolyte (being the electrolytic solution in the electrolyzer), owing to be subjected to the membranous obstruction of crucible, Au 3+Can not enter catholyte (being in the electrolytic solution in the unglazed crucible), and H +, Cl -Can freely pass through.No gold is separated out and releasing hydrogen gas only on the negative electrode like this, Au 3+Just in anolyte, gather, can make the solution that contains golden 100 grams per liters~400 grams per liters at last.This solution purifies gold solution through filtering, and controls solution temperature in reactor, and with the pH value of sodium hydroxide adjustment solution, reduce with reductive agent PH=-1~5 again.
The reductive agent of the inventive method is oxalic acid, S-WAT, Sodium Pyrosulfite, acetate, sulfurous gas or ferrous salt; Consumption is 1~2 times of stoichiometric ratio.
Optionally reduce gold by gold ion concentration in the sampling and measuring solution or the redox potential of measuring solution in the inventive method reduction process, according to foreign matter content height in the gold solution, the reduction ratio of control gold generally is controlled between 70~99%.
After stopping reduction reaction, filter the bronze restore in strainer, the washing that water is careful obtains the 1# bronze of national regulation.
In the above-mentioned reduction process, temperature of reaction is 40~90 ℃, by settling bath or the outer steam jacket heating of reactor.
The thick gold of above-mentioned raw material is: the thick gold that contains gold 85~99.5% grades.
The present invention has following excellent results:
One, compare with refining, thick gold grade scope is relaxed, and the adaptability of raw material is strengthened greatly; Flow process overstocks and significantly reduces.
Two, compare with the efflorescence purification, reduced technological process, merge into one step of electrochemical dissolution by original thick bronzeization, chemical dissolution; Home-made equipment has been saved investment greatly; Production cost is purified than efflorescence and is reduced greatly.
(4) embodiment
Embodiment 1.
Contain the thick gold of golden 90% grade, cast positive plate, make negative electrode with proof gold, carry out electrolysis with dilute hydrochloric acid as electrolytic solution, electrolyzer is a ceramic trough, and negative electrode is made barrier film with the biscuit ware crucible.Electrolytic solution dilute hydrochloric acid is HCl in the above-mentioned electrolyzer: H 2O=2: 1, electrolytic solution dilute hydrochloric acid is HCl in the crucible: H 2O=1: 1.Liquid level is higher than electrolyzer liquid level 8mm in the crucible.The control pulsatory current, make golden electrochemical solution, gold solution concentration reaches 250 grams per liters, after the filtration, controls solution temperature in reactor, adjust the pH value of solution with sodium hydroxide, PH=0, with the reductive agent reduction, reductive agent is the oxalic acid of 1.2 times of stoichiometric ratios, temperature of reaction is 60 ℃, is heated by settling bath.Reaction finishes, and filtration washing obtains bronze.Sampling reaches more than 99.95% with the fire assay gold content, and 6 impurity elements using ICP assay national regulation then are in the 1# of national regulation lsp request scope.
Embodiment 2.
Contain the thick gold of golden 99% grade, cast positive plate, make negative electrode with the titanium plate, carry out electrolysis with dilute hydrochloric acid as electrolytic solution, electrolyzer is a ceramic trough, and negative electrode is made barrier film with the biscuit ware crucible.Electrolytic solution dilute hydrochloric acid is HCl in the above-mentioned electrolyzer: H 2O=1.8: 1, electrolytic solution dilute hydrochloric acid is HCl in the crucible: H 2O=1.2: 1.Liquid level is higher than electrolyzer liquid level 10mm in the crucible.The control pulsatory current, make golden electrochemical solution, gold solution concentration reaches 300 grams per liters, after the filtration, controls solution temperature in reactor, adjust the pH value of solution with sodium hydroxide, PH=1, with the reductive agent reduction, reductive agent is the S-WAT of 1.1 times of stoichiometric ratios, temperature of reaction is 50 ℃, by the outer steam jacket heating of reactor.Reaction finishes, and filtration washing obtains bronze.Sampling reaches more than 99.95% with the fire assay gold content, and 6 impurity elements using ICP assay national regulation then are entirely in the 1# of national regulation lsp request scope.
Embodiment 3.
Contain the thick gold of golden 85% grade, cast positive plate, make negative electrode with proof gold, carry out electrolysis with dilute hydrochloric acid as electrolytic solution, electrolyzer is a ceramic trough, and negative electrode is made barrier film with the biscuit ware crucible.Electrolytic solution dilute hydrochloric acid is HCl in the above-mentioned electrolyzer: H 2O=2.5: 1, electrolytic solution dilute hydrochloric acid is HCl in the crucible: H 2O=1: 1.2.Liquid level is higher than electrolyzer liquid level 6mm in the crucible.The control pulsatory current makes golden electrochemical solution, and gold solution concentration reaches 200 grams per liters, after the filtration, in reactor, control solution temperature, with the pH value of sodium hydroxide adjustment solution, PH=3, with the reductive agent reduction, reductive agent is the acetate of 1.3 times of stoichiometric ratios, and temperature of reaction is 55 ℃.Reaction finishes, and filtration washing obtains bronze.Sampling reaches more than 99.95% with the fire assay gold content, and 6 impurity elements using ICP assay national regulation then are entirely in the 1# of national regulation lsp request scope.
Embodiment 4. is as described in the embodiment 1, and different is that electrolyzer is a plastic channel.

Claims (10)

1. the method that thick gold is purified comprises the thick gold of raw material is cast as Jinyang pole plate, and electrochemical solution makes gold be converted into gold solution, and control solution Gold Content or controlled oxidation reduction potential are reduced to the 1# bronze with reductive agent with gold solution.
2. the method that thick gold as claimed in claim 1 is purified is characterized in that electrochemical solution is to make negative electrode with proof gold or titanium plate, carries out electrolysis with dilute hydrochloric acid as electrolytic solution, and electrolyzer is pottery or plastic channel, and negative electrode is made barrier film with the biscuit ware crucible.
3. the method that thick gold as claimed in claim 1 or 2 is purified is characterized in that electrolytic solution dilute hydrochloric acid is HCl in the electrolyzer: H 2O=1.5~3: 1, electrolytic solution dilute hydrochloric acid is HCl in the crucible: H 2O=1~2: 1~2.
4. the method that thick gold as claimed in claim 1 or 2 is purified is characterized in that liquid level is higher than electrolyzer liquid level 5~10mm in the described crucible.
5. the method that thick gold as claimed in claim 1 is purified is characterized in that, feeds pulsatory current, the thick gold dissolving of anode makes the solution that contains golden 100 grams per liters~400 grams per liters, filters, control solution temperature in reactor, the pH value with sodium hydroxide adjustment solution reduces with reductive agent again.
6. as the method for claim 1 or 5 described thick gold purifications, it is characterized in that described reductive agent is oxalic acid, S-WAT, Sodium Pyrosulfite, acetate, sulfurous gas or ferrous salt, consumption is 1~2 times of stoichiometric ratio.
7. the method that thick gold as claimed in claim 1 is purified is characterized in that, optionally reduces gold by gold ion concentration in the sampling and measuring solution or the redox potential of measuring solution in the reduction process, the reduction ratio 70~99% of control gold.
8. the method that thick gold as claimed in claim 1 is purified is characterized in that, after reduction reaction is finished, filters the bronze that restores in strainer, washes with water, obtains the 1# bronze.
9. the method that thick gold as claimed in claim 1 is purified is characterized in that in the described reduction process, temperature of reaction is 40~90 ℃, by settling bath or the outer steam jacket heating of reactor.
10. the method that thick gold as claimed in claim 1 is purified is characterized in that the thick gold of described raw material is the thick gold that contains gold 85~99.5% grades.
CN 03112144 2003-04-11 2003-04-11 Method of crude gold purification Expired - Fee Related CN1208482C (en)

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CN1208482C CN1208482C (en) 2005-06-29

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102021340A (en) * 2010-12-04 2011-04-20 金川集团有限公司 Deep impurity removal technology for coarse gold powder
CN106756047A (en) * 2016-12-23 2017-05-31 郴州市金贵银业股份有限公司 Debris silver anode slime high puies forward the processing method of gold
CN106868545A (en) * 2017-01-12 2017-06-20 包小玲 Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low
CN107460324A (en) * 2017-08-23 2017-12-12 中南大学 A kind of method that silver anode slime control current potential prepares four or nine gold medals
CN109312481A (en) * 2016-03-09 2019-02-05 托尔斯滕·科拉斯公司 The electrorefining of thick gold
CN110205500A (en) * 2019-06-18 2019-09-06 山东黄金冶炼有限公司 The removal methods of impurity in a kind of reduction bronze

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102021340A (en) * 2010-12-04 2011-04-20 金川集团有限公司 Deep impurity removal technology for coarse gold powder
CN102021340B (en) * 2010-12-04 2013-01-09 金川集团有限公司 Deep impurity removal technology for coarse gold powder
CN109312481A (en) * 2016-03-09 2019-02-05 托尔斯滕·科拉斯公司 The electrorefining of thick gold
CN109312481B (en) * 2016-03-09 2020-10-16 托尔斯滕·科拉斯公司 Electrolytic purification of crude gold
CN106756047A (en) * 2016-12-23 2017-05-31 郴州市金贵银业股份有限公司 Debris silver anode slime high puies forward the processing method of gold
CN106756047B (en) * 2016-12-23 2018-06-29 郴州市金贵银业股份有限公司 High sundries silver anode slime puies forward the processing method of gold
CN106868545A (en) * 2017-01-12 2017-06-20 包小玲 Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low
CN107460324A (en) * 2017-08-23 2017-12-12 中南大学 A kind of method that silver anode slime control current potential prepares four or nine gold medals
CN110205500A (en) * 2019-06-18 2019-09-06 山东黄金冶炼有限公司 The removal methods of impurity in a kind of reduction bronze
CN110205500B (en) * 2019-06-18 2021-09-17 山东黄金冶炼有限公司 Method for removing impurities in reduced gold powder

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Owner name: SHANDONG GOLD MINE CO., LTD.

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Address after: No. 609, Laizhou North Road, Laizhou, Shandong

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Granted publication date: 20050629

Termination date: 20130411