CN102071323A - Method for producing high-purity gold by utilizing electroplating waste liquid containing gold - Google Patents
Method for producing high-purity gold by utilizing electroplating waste liquid containing gold Download PDFInfo
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- CN102071323A CN102071323A CN 201010614136 CN201010614136A CN102071323A CN 102071323 A CN102071323 A CN 102071323A CN 201010614136 CN201010614136 CN 201010614136 CN 201010614136 A CN201010614136 A CN 201010614136A CN 102071323 A CN102071323 A CN 102071323A
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Abstract
The invention relates to a method for producing high-purity gold by utilizing electroplating waste liquid containing gold. The electroplating waste liquid containing gold is taken as an object, and the method comprises the following steps of: electrolyzing the electroplating waste liquid containing gold by using an electrolysis machine to obtain coarse gold mud; primarily removing impurities from the coarse gold mud obtained through electrolysis, and filtering and washing to obtain gold mud; dissolving the gold mud, and filtering and washing to obtain gold-containing solution; adding a reducing agent into the gold-containing solution to reduce gold; secondarily removing impurities from the gold mud obtained through reduction to obtain pure gold mud; and drying and casting the pure gold mud into ingots. Through the method, the gold recovery rate is over 99 percent, and the gold purity is stabilized over 99 percent. The method is convenient to operate, and low in investment and production cost, and has good social and economic benefits.
Description
Technical field
The present invention relates to the waste liquid metal recovery processes, specifically a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing.
Background technology
Prosperity development along with industries such as gold-plated jewellery, gold-plated goods, thereby produced a large amount of plating and contained golden waste liquid, if the gold that plating is contained in the golden waste liquid is not recycled, will cause huge waste to limited gold resource, also can cause bad influence simultaneously to environment.Therefore, plating is contained golden waste liquid and carry out that comprehensive resource is recycled and harmlessness disposing will produce long-range economic benefit and social benefit.
In recent years, the comprehensive reutilization scholars both domestic and external that contain gold in the golden waste liquid for plating have done many research work in this respect, have also obtained the achievement of many stages.
" the gold extraction method in the gold electroplating effluent " that Chinese patent CN1243890A discloses, it is characterized in that by add red ketone salt to the gold electroplating effluent, sulfuric acid, in waste liquid, produce precipitation, leave standstill throw out, getting wherein, throw out adds Wingdale (or caustic soda) in succession, zinc powder, borax fully stir roasting, the roasting postcooling is taken bottom, and removing slag with ash blowing method to get the ingot of wanting.The main drawback that this technology exists is the operational condition harshness, and roasting time is long, and energy consumption is big, the cost height.
" cultural method of granule sludge and utilize it from contain golden waste liquid, to reclaim the method for gold " that Chinese patent CN1872992A discloses, it is characterized in that in containing golden waste liquid, adding the granule sludge of special cultivation, be positioned in the constant temperature shaking table, after fully adsorbing, gravity settling, the supernatant liquor after the sedimentation inclines and, continuing to add granule sludge adsorbs by above-mentioned condition, add desorbing agent solution in the precipitation and carry out desorption, behind the gravity settling, in desorption liquid, add the displacement metal and can obtain gold.Operational condition required height when this technology existed main drawback to be particle cultivation and particle absorption, and process cycle is long, and difficulty realizes industrialization.
The Hiroshima University of Japan work out a kind of from contain golden waste liquid the novel method of high efficiente callback gold.This method utilizes complex compound that metal ion is had the selection adsorptivity.Its technological process is to add the ring polyamino compound that is dissolved in the trichloromethane in the pH value is strongly-acid gold mixed solution below 1, stir half an hour after, gold and cyclic polyamine compound are fully reacted, generate golden complex compound.This complex compound and other metal mixed solution are divided into up and down in reaction vessel, and two-phase exists.After gold complex taken out, it is heated to 60 ℃, in pH value is 8 neutrality or weak alkaline aqueous solution, stirs half an hour, gold complex is because structural instability is divided into golden and two kinds of materials of polyamine again.Gold and polyamine solution still exist with the two-phase form, and the gold on the top that remains in reactor is reclaimed.The main drawback of this technology is exactly that the Jin Shihui that is used for reclaiming the gold-plated waste liquid of cyaniding produces deleterious HCN gas.
Summary of the invention
Technical problem to be solved: the object of the invention is to overcome the shortcoming that above technology exists, and provides a kind of the utilization to electroplate the method that contains golden waste liquid production High Purity Gold, and production cost is low, the gold recovery height.
Technical scheme: for achieving the above object, a kind of utilization of the present invention electroplated the method that contains golden waste liquid production High Purity Gold, and containing golden waste liquid with plating is object, and its method comprises successively:
(A), electroplate and to contain golden waste liquid and separate with electrolysis electromechanics and obtain thick gold mud;
(B), a removal of impurities of the thick gold mud of electrolysis, filtration washing gets gold mud;
(C), the molten gold of gold mud, filtration washing gets gold-containing solution;
(D), gold-containing solution adds reductive agent reduction gold;
(E), will reduce the removal of impurities of gained gold mud secondary gets proof gold mud;
(F), with the oven dry of proof gold mud, ingot casting.
In the such scheme: described plating contains golden waste liquid and is meant that mainly the plating that contains copper, iron, nickel, zinc, chromium, silver, potassium, one or more metallic impurity of sodium contains golden waste liquid.Described electrolysis machine adopts is that the empty cylindrical carbon fiber rod more than three of periodic replacement is made negative electrode, and the batch cycle electrolysis mode carries out electrolysis, when gold content in the lean electrolyte is reduced to 0.5mg/L end electrolysis when following.Described " removal of impurities of the thick gold mud of electrolysis " is to be that 10%～37% hydrochloric acid is 70 ℃～90 ℃ of temperature with the nitric acid of concentration 30%～98% or concentration, L/S=3～6: 1, carry out under time 1h～3h condition, the removal of impurities number of times is 1～2 time, and the gold mud after the removal of impurities filters and washing.Described " the molten gold of gold mud " be with chloroazotic acid L/S=3～6: 1, time 1h～3h carries out under 50 ℃～80 ℃ conditions, molten gold finishes after-filtration and washing.Described reductive agent is any in hydrazine hydrate, S-WAT, the oxalic acid.Described gold-containing solution adds reductive agent reduction gold, and the reductive agent consumption is 1～4 times of theoretical amount, time 1h～3h, 50 ℃～60 ℃ of temperature or room temperature.Described " removal of impurities of reduction gained gold mud secondary " is also to filter to neutral with hot wash earlier, uses analytical pure nitric acid or salt acid elution 2～3 times then, removes by filter metallic impurity, and last reusable heat water washing is to neutral.
Unusual effect of the present invention is: the present invention utilizes to electroplate and contains golden waste liquid recovery gold, and rate of recovery height reclaims Jin Keda more than 99%, and the purity of gold is stabilized in more than 99%.Good product quality of the present invention, equipment is simple, and is easy to operate, less investment, production cost is low, is easy to suitability for industrialized production, has good social benefit and economic benefit.
Description of drawings
Fig. 1 is the invented technology schema.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiments of the invention, but can not limit protection scope of the present invention with this.
Embodiment 1
(1) plating contains golden waste liquid electrolysis
Plating contains golden waste liquid and carries out the batch cycle electrolysis with electrolysis machine, timing sampling analysis in the electrolytic process, reduce to 0.5mg/L when gold content in the lean electrolyte and finish the electrolysis that this batch plating contains golden waste liquid when following, changing new plating again contains golden waste liquid and continues electrolysis and carry gold, take out negative electrode after the negative electrode gold content runs up to some amount, the negative electrode that more renews is proceeded electrolysis.
(2) removal of impurities of the thick gold mud of electrolysis
To contain golden carbon fiber cathode bar handles to thin piece, be added in the enamel reaction still then, industrial nitric acid with 60%, at 85 ℃, react 1.5h under the L/S=4 condition, question response carries out filtration washing after finishing, and reactor keeps negative pressure in the reaction process, the waste gas that produces absorbs with Tower for purifying waste gas to be handled, and the waste water of generation send Waste Water Treatment to handle to back up to standard discharging.
(3) the molten gold of gold mud
Gold mud after the removal of impurities is placed enamel reaction still, carrying out filtration washing after with L/S=3 aqua regia dissolution 1.5h under 70 ℃ of conditions, reactor keeps negative pressure in the reaction process, and the waste gas of generation absorbs with Tower for purifying waste gas to be handled, the filter residue that produces is discarded, and gold-containing solution keeps stand-by.
(4) reduction
Gold-containing solution reduces 1.5h with the S-WAT of 3 times of theoretical aequums under 50 ℃ of conditions in enamel reaction still, the gold mud that restores filters.Reactor keeps negative pressure in the reaction process, and the waste gas of generation absorbs with Tower for purifying waste gas to be handled, and the waste water of generation send Waste Water Treatment to handle to back up to standard discharging.
(5) secondary removal of impurities
The gold mud that restores repeats filtration washing to neutral with hot water earlier, carries out washing and filtering 2 times with analytical pure nitric acid then, and last reusable heat water repeats filtration washing to neutrality and obtains proof gold mud.
(6) oven dry
Place pure titanium dish on electric furnace, to dry in proof gold mud.
(7) ingot casting
Gold mud after the oven dry is put in carries out melting in the intermediate frequency furnace under 1200 ℃, then Jinsui River is poured into ingot casting obtains the finished product ingot in the mold.
The recovery Jin Keda of present embodiment is more than 99.9%, and the purity of gold is stabilized in more than 99.95%.
Embodiment 2
Plating contains that golden waste liquid electrolysis obtains thick gold mud, reduction gold mud oven dry is identical with embodiment 1 with the ingot casting operation, and other operation technical qualification are as follows:
(1) removal of impurities of the thick gold mud of electrolysis
The thick gold mud of electrolysis once removes and uses mixedly 10% technical hydrochloric acid, at 70 ℃, reacts 3h under the L/S=6 condition.
(2) the molten gold of gold mud
Gold mud after the removal of impurities places reactor, uses L/S=6 aqua regia dissolution 1h under 50 ℃ of conditions.
(3) reduction
Gold-containing solution reduces 1h at ambient temperature with the hydrazine hydrate of 3 times of theoretical aequums in reactor.
(4) secondary removal of impurities
The gold mud that restores repeats filtration washing to neutral with hot water earlier, carries out washing and filtering 3 times with analytical pure hydrochloric acid then, and last reusable heat water repeats filtration washing to neutrality and obtains proof gold mud.Present embodiment reclaims Jin Keda more than 99%, and the purity of gold is stabilized in more than 99.9%.
Embodiment 3
Plating contains that golden waste liquid electrolysis obtains thick gold mud, the removal of impurities of reduction gold mud secondary, the oven dry of reduction gold mud is identical with embodiment 1 with the ingot casting operation, and other operation technical qualification are as follows:
(1) removal of impurities of the thick gold mud of electrolysis
The thick gold mud of electrolysis once removes and uses mixedly 30% industrial nitric acid, at 90 ℃, reacts 3h under the L/S=4 condition.
(2) the molten gold of gold mud
Gold mud after the removal of impurities places reactor, uses L/S=4 aqua regia dissolution 1h under 80 ℃ of conditions.
(3) reduction
Gold-containing solution reduces 3h with the oxalic acid of 4 times of theoretical aequums under 60 ℃ of conditions in reactor.
Present embodiment reclaims Jin Keda more than 99%, and the purity of gold is stabilized in more than 99%.
Claims (8)
1. a method of utilizing plating to contain golden waste liquid production High Purity Gold is characterized in that containing golden waste liquid with plating is object, and its method comprises successively:
(A), electroplate and to contain golden waste liquid and separate with electrolysis electromechanics and obtain thick gold mud;
(B), a removal of impurities of the thick gold mud of electrolysis, filtration washing gets gold mud;
(C), the molten gold of gold mud, filtration washing gets gold-containing solution;
(D), gold-containing solution adds reductive agent reduction gold;
(E), will reduce the removal of impurities of gained gold mud secondary gets proof gold mud;
(F), with the oven dry of proof gold mud, ingot casting.
2. a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing according to claim 1, it is characterized in that described plating contains golden waste liquid and is meant that mainly the plating that contains copper, iron, nickel, zinc, chromium, silver, potassium, one or more metallic impurity of sodium contains golden waste liquid.
3. a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing according to claim 1, it is characterized in that, what described electrolysis machine adopted is that the empty cylindrical carbon fiber rod more than three that regularly replaces is made negative electrode, the batch cycle electrolysis mode carries out electrolysis, reduces to 0.5mg/L when gold content in the lean electrolyte and finishes electrolysis when following.
4. a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing according to claim 1, it is characterized in that, described " removal of impurities of the thick gold mud of electrolysis " is to be that 10%～37% hydrochloric acid is 70 ℃～90 ℃ of temperature with the nitric acid of concentration 30%～98% or concentration, L/S=3～6: 1, carry out under time 1h～3h condition, the removal of impurities number of times is 1～2 time, and the gold mud after the removal of impurities filters and washing.
5. a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing according to claim 1, it is characterized in that described " the molten gold of gold mud " is at L/S=3～6: 1, time 1h～3h with chloroazotic acid, carry out under 50 ℃～80 ℃ conditions, molten gold finishes after-filtration and washing.
6. a kind of utilization the according to claim 1 electroplated the method that contains golden waste liquid production High Purity Gold, it is characterized in that described reductive agent is any in hydrazine hydrate, S-WAT, the oxalic acid.
7. a kind of utilization the according to claim 1 electroplated the method that contains golden waste liquid production High Purity Gold, it is characterized in that, described gold-containing solution adds reductive agent reduction gold, and the reductive agent consumption is 1～4 times of theoretical amount, time 1h～3h, 50 ℃～60 ℃ of temperature or room temperature.
8. a kind of method that contains golden waste liquid production High Purity Gold of electroplating of utilizing according to claim 1, it is characterized in that, described " removal of impurities of reduction gained gold mud secondary ", be also to filter to neutral with hot wash earlier, use analytical pure nitric acid or salt acid elution 2～3 times then, remove by filter metallic impurity, extremely neutral with hot wash at last.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194770A (en) * | 2013-03-22 | 2013-07-10 | 紫金矿业集团股份有限公司 | Process for extracting gold from low-grade, copper-containing and difficultly-treated goldmine ammonia cyanide leaching pulp via electrodeposition |
| CN104047024A (en) * | 2014-07-09 | 2014-09-17 | 苏州东吴黄金文化发展有限公司 | Process for preparing high-purity gold by primary electrolytic refining |
| CN105463195A (en) * | 2015-12-04 | 2016-04-06 | 无锡英特派金属制品有限公司 | Purification method for gold in gold-nickel alloy |
| CN103572322B (en) * | 2012-08-02 | 2017-05-10 | 厦门紫金矿冶技术有限公司 | Method for recycling gold and copper from copper-containing oxidization gold ores |
| CN109055983A (en) * | 2018-06-13 | 2018-12-21 | 珠海格力电器股份有限公司 | A kind of recovery process and device of the plating containing golden waste water |
| CN111778519A (en) * | 2020-05-20 | 2020-10-16 | 金川集团股份有限公司 | Method for digesting solid impurity elements of lead, zinc and selenium in nickel electrolytic solution |
| CN114277257A (en) * | 2021-11-29 | 2022-04-05 | 昆山鸿福泰环保科技有限公司 | Method for recovering gold from gold-containing waste liquid |
Families Citing this family (1)
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| CN105350017B (en) * | 2015-11-30 | 2017-05-03 | 长春黄金研究院 | Method increasing rate of filtration of desorbed and electrolyzed gold mud |
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| CN1271781A (en) * | 1999-04-22 | 2000-11-01 | 中南工业大学 | Process for preparing gold by reduction of gold-contained chlorated liquid |
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Patent Citations (3)
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| CN1271781A (en) * | 1999-04-22 | 2000-11-01 | 中南工业大学 | Process for preparing gold by reduction of gold-contained chlorated liquid |
| CN101037285A (en) * | 2007-02-09 | 2007-09-19 | 苏州市环境工程有限责任公司 | Integrative recovering and reusing of heavy metals in wire board plating wastewater treatment sludge |
| CN101328541A (en) * | 2008-07-27 | 2008-12-24 | 郴州市金贵银业股份有限公司 | Gold wet purification process |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103572322B (en) * | 2012-08-02 | 2017-05-10 | 厦门紫金矿冶技术有限公司 | Method for recycling gold and copper from copper-containing oxidization gold ores |
| CN103194770A (en) * | 2013-03-22 | 2013-07-10 | 紫金矿业集团股份有限公司 | Process for extracting gold from low-grade, copper-containing and difficultly-treated goldmine ammonia cyanide leaching pulp via electrodeposition |
| CN103194770B (en) * | 2013-03-22 | 2016-03-09 | 紫金矿业集团股份有限公司 | From low-grade cupric difficult-treating gold mine ammonia-cyanide leaching ore pulp, electrodeposition puies forward the technique of gold |
| CN104047024A (en) * | 2014-07-09 | 2014-09-17 | 苏州东吴黄金文化发展有限公司 | Process for preparing high-purity gold by primary electrolytic refining |
| CN105463195A (en) * | 2015-12-04 | 2016-04-06 | 无锡英特派金属制品有限公司 | Purification method for gold in gold-nickel alloy |
| CN109055983A (en) * | 2018-06-13 | 2018-12-21 | 珠海格力电器股份有限公司 | A kind of recovery process and device of the plating containing golden waste water |
| CN109055983B (en) * | 2018-06-13 | 2023-08-22 | 珠海格力电器股份有限公司 | Recovery process and device for electroplating gold-containing wastewater |
| CN111778519A (en) * | 2020-05-20 | 2020-10-16 | 金川集团股份有限公司 | Method for digesting solid impurity elements of lead, zinc and selenium in nickel electrolytic solution |
| CN111778519B (en) * | 2020-05-20 | 2022-05-31 | 金川集团股份有限公司 | Method for digesting solid impurity elements of lead, zinc and selenium in nickel electrolytic solution |
| CN114277257A (en) * | 2021-11-29 | 2022-04-05 | 昆山鸿福泰环保科技有限公司 | Method for recovering gold from gold-containing waste liquid |
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