CN101805080A - New technology for recycling valuable elements in biological oxidation gold extraction liquid - Google Patents
New technology for recycling valuable elements in biological oxidation gold extraction liquid Download PDFInfo
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- CN101805080A CN101805080A CN 201010121194 CN201010121194A CN101805080A CN 101805080 A CN101805080 A CN 101805080A CN 201010121194 CN201010121194 CN 201010121194 CN 201010121194 A CN201010121194 A CN 201010121194A CN 101805080 A CN101805080 A CN 101805080A
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Abstract
The invention discloses new technology for recycling valuable elements in biological oxidation gold extraction liquid. The technology comprises the following steps: simultaneously adding acid arsenic-containing biological oxidation gold extraction waste liquid and a phosphate radical-containing precipitator (acid or salt) into a reaction kettle and performing selective precipitation to realize arsenic and iron separation; realizing solid-liquid separation by using filtering technology, allowing a solid phase to enter an iron phosphate preparation process and allowing liquid to enter an arsenic recycling and copper arsenate preparing process; precipitating solution from which arsenic is recycled and lime milk; drying solid-phase calcium sulfate to obtain a building material product after solid-liquid separation, wherein the liquid phase is ammonia ion-containing alkaline solution; and returning to a primary biological oxidation gold extraction process to realize zero discharge in whole flow. The new technology has the advantages of realizing effective separation of arsenic and iron in the acid arsenic-containing biological oxidation gold extraction waste liquid, preparing arsenic, iron and sulfur products with high additional values, achieving zero discharge in the whole flow and no secondary pollution, and realizing hazard-free and resource comprehensive treatment of the acid arsenic-containing biological oxidation gold extraction waste liquid.
Description
Technical field
The present invention relates to from acidic arsenic-containing biological oxidation gold extraction waste liquor, extract a kind of technology of valuable element.
Background technology
How tame the at present domestic factory that has built up employing biological oxidation gold extraction technology has, and becomes and has maximum country of biological oxidation gold extraction factory in the world.
But, producing a large amount of arsenic-containing acid biological oxidation gold extraction waste liquors in the biological oxidation gold extraction technology, this class biological oxidation solution pH value 0.6～1.8 is according to the mineral composition and the oxidizing condition difference of the raw mineral materials of handling, every m
3Oxidation liquid can contain oligo-elementss such as arsenic about (25-45) kg iron and 8kg and copper, zinc, lead.The compound of arsenic is a kind of protoplasma poisonous substance, has biological effect widely, is defined as first kind carcinogens by world anti-cancer research institution.
Handle at present acidic arsenic-containing biological oxidation gold extraction waste liquor comparatively successful method be " lime iron salt method ", promptly Fe/As greater than 3 condition under, carry out neutralizing treatment with lime, make the more stable FeAsO of As generation
4Precipitation is removed from solution.But carry gold at biological oxidation solution and also have Fe in useless
2+, cause the arsenic of " in and slag " lining can not be fully with FeAsO
4Exist, but part is with Ca (AsO
3)
2Form exist.The arsenical salt of this class is with the variation of edaphic condition, the effect of bacterium in addition, and solubleness increases, and can cause tangible secondary pollution.Main is to adopt " lime molysite neutralization precipitation method " when carrying out harmless treatment, need to consume a large amount of lime, handle 1 ton of gold ore and consume lime 300～400Kg, if day 100 tons of gold ore of processing, the biological oxidation gold extraction waste liquor that produces is with " lime iron salt method " when carrying out harmless treatment, then need 30～40 tons in daily consumption lime, and in about the generation hundredweight and slag, so annual then produce about 40,000 tons in and slag, the quantity of slag is so big, outward transport will expend a large amount of manpowers, financial resources, increases the gold production cost.In addition, these contain in the arsenic and slag is put in the mine tailing storehouse, also are the potential source of pollution.Simultaneously, valuable elements such as the arsenic in the acidic arsenic-containing biological oxidation gold extraction waste liquor, iron, sulphur are thrown away again in vain.Day is handled the day acid discharge biological oxidation gold extraction waste liquor 500-600m of biological oxidation gold extraction factory of 100 tons of gold ore
3, throw away nearly 1400～1700 tons of arsenic and 4000-8000 ton iron every year in vain, cause the very big wasting of resources.These valuable elements to be reclaimed, make high value-added product, can produce considerable economic.
Summary of the invention
Weak point at existing acid biological oxidation gold extraction waste liquor treatment technology, the invention provides a kind of is support with the chemical method, be aided with outer field action, from acidic arsenic-containing biological oxidation gold extraction waste liquor, reclaim valuable element and prepare the method for high value added product, present method can make acidic arsenic-containing biological oxidation gold extraction waste liquor reach innoxious, and realize comprehensive utilization of resources and gold Production Flow Chart zero release reducing the gold production cost, increase economic efficiency.
The present invention is for solving acid biological oxidation gold extraction waste liquor treatment technology problem, the technical scheme that is adopted is: acidic arsenic-containing biological oxidation gold extraction waste liquor is as process object, contain elements such as Fe, As, Zn, Cu, Pb, S in this waste liquid, its content is respectively 25～45gL
-1Fe, 2～9gL
-1As, 0.1～0.3gL
-1Zn, 0.01～0.07gL
-1Cu, 0.02～0.03gL
-1Pb, 12～30gL
-1S, wherein sulphur and arsenic exist with the form of sulfate radical and arsenate respectively, and the iron majority is with Fe
3+Form exists, biological oxidation gold extraction waste liquor pH value 0.6～1.8.
In view of above-mentioned condition, the technological process of extracting valuable element is:
1) add acidic arsenic-containing biological oxidation gold extraction waste liquor and ammonium dibasic phosphate solution, simultaneously in reactor (a), its concentration is 2molL
-1Also can be primary ammonium phosphate or triammonium phosphate, by ammoniacal liquor or phosphoric acid control reactor internal reaction system pH be 1.5～2.5, under the condition of 75 ℃～90 ℃ of temperature of reaction, stirring intensity 600～800rpm/min by selective precipitation, realize that arsenic iron separates;
If adopting triammonium phosphate is precipitation agent, principal reaction is Fe
3++ PO
4 3-=FePO
4↓
2), adopt to filter or after technology such as centrifugation realized solid-liquid separation, the solid phase precipitation thing entered the preparation section of tertiary iron phosphate, liquid enters the preparation section of arsenic product;
3), iron precipitate is through washing 3～5 times, aged at room temperature 10h～12h, after drying 6～8 hours under air atmosphere, 80～120 ℃ of conditions of temperature, roasting 8h～10h under 500 ℃～700 ℃ conditions of temperature obtains the tertiary iron phosphate product;
4), to reactor (b) in, add simultaneously pass through after the solid-liquid separation contain arsenic liquid and concentration is 1molL
-1Copper-bath adopts ammoniacal liquor to regulate under pH value 3～7, the stirring intensity 300～500rpm/min condition, prepares the cupric arsenate throw out by precipitin reaction;
Copper sulfate is 3Cu with containing the principal reaction that the arsenic tail washings takes place after arsenic iron separates
2++ 2AsO
4 3-=Cu
3(AsO
4)
2↓
5), the cupric arsenate throw out is through washing 3～5 times, aged at room temperature 2h～5h, after drying 3～5 hours under air atmosphere, 60～80 ℃ of conditions of temperature, roasting 6h～8h under 350 ℃～450 ℃ conditions of temperature obtains the cupric arsenate product;
6), simultaneously add tail washings and lime slurry after reclaiming arsenic, under control pH value of solution value 7～10 conditions, under the condition of 25 ℃～80 ℃ of temperature, stirring intensity 600～800rpm/min, obtain calcium sulfate precipitation by selective precipitation to reactor (c);
7), adopt to filter or centrifugal separation technique is realized solid-liquid separation, make building material product after separating back solid phase calcium sulfate oven dry, liquid returns the protista oxidation and puies forward the metal working preface, realizes the whole process zero release.
The invention has the beneficial effects as follows:
1, the arsenic, iron of realizing acidic arsenic-containing biological oxidation gold extraction waste liquor effectively separation and arsenic, iron, sulphur content do not recycle, the rate of recovery of arsenic, iron, sulphur is equal more than 98%;
2, prepare market and use tertiary iron phosphate, cupric arsenate and calcium sulfate product preferably;
3, whole process zero release, non-secondary pollution;
4, acidic arsenic-containing biological oxidation gold extraction waste liquor is realized innoxious, recycling comprehensive treatment, makes the technology of " biological oxidation gold extraction technology " more perfect.Avoid in the former technology " lime iron salt method " to handle that acidic arsenic-containing biological oxidation gold extraction waste liquor lime consumption amount is big, the quantity of slag big, potential pollution source is arranged, throw away valuable element in vain causes shortcomings such as the wasting of resources.
Description of drawings
Fig. 1 is the process flow sheet that extracts valuable element from acidic arsenic-containing biological oxidation gold extraction waste liquor;
Embodiment
Example 1
1, to handle 250m every day
3Biological oxidation gold extraction waste liquor (principal element Fe content is 24g/L, and As content is 5g/L) is an example, and the recovery technological process of its valuable element is: Secondary ammonium phosphate is a precipitation agent, is made into 2molL
-1Ammonium dibasic phosphate solution, to reactor (a) in, add simultaneously acidic arsenic-containing biological oxidation gold extraction waste liquor and precipitant solution, adjustment bio-oxidation flow velocity is 10.5m
3/ h, the precipitant solution flow velocity is about 5.6m
3/ h adjusts the precipitation agent flow velocity at any time, pH=1.5 ± 0.2 in the control reactor, and 75 ℃ of temperature of reaction, stirring intensity 800rpm/min carries out arsenic iron to be separated;
2, adopt filtration or centrifugal separation technique, carry out solid-liquid separation, solid phase enters the tertiary iron phosphate preparation section, contains arsenic liquid and enters arsenic product preparation operation;
3, the washing of solid phase precipitation thing is 3 times, and aged at room temperature 12h behind air atmosphere, 80 ℃ of oven dry of the temperature 8h, at air atmosphere, 500 ℃ of roasting 10h, obtains the tertiary iron phosphate product;
4, gained contains arsenic liquid and enters the arsenic recovery process: will contain arsenic liquid, 1molL
-1Three kinds of liquid of the copper sulfate of concentration, ammoniacal liquor simultaneously and stream join in the reactor (b), containing arsenic liquid bare flow is 15m
3/ h contains arsenic liquid: the copper sulfate velocity ratio is controlled to be 10: 1, suitably adjusts the flow velocity of ammoniacal liquor, pH=3 ± 0.2 in the control reaction system, stirring intensity 300rpm/min carries out the cupric arsenate precipitation, the liquid that flows out from reactor passes through solid-liquid separation, obtains the throw out of cupric arsenate;
5, the washing of cupric arsenate throw out is 3 times, aged at room temperature 5h, and after 5 hours, 350 ℃ of roasting 8h obtain the cupric arsenate product in air atmosphere, 60 ℃ of oven dry;
6, solution and the lime slurry of while after reactor (c) adds recovery arsenic under pH value of solution=7 ± 0.2 conditions, obtains calcium sulphate solid by selective precipitation in the control still under the condition of 70 ℃ of temperature, stirring intensity 800rpm/min;
7, adopt filtration or centrifugal separation technique to realize solid-liquid separation, make building material product after the solid phase oven dry; Liquid returns the protista oxidation and puies forward the metal working preface, realizes the whole process zero release.
Example 2
1, to handle 300m every day
3Biological oxidation gold extraction waste liquor (principal element Fe content is 36g/L, and As content is 7.5g/L) is an example, and the recovery technological process of its valuable element is: Secondary ammonium phosphate is a precipitation agent, is made into 2molL
-1Ammonium dibasic phosphate solution, to reactor (a) in, add simultaneously acidic arsenic-containing biological oxidation gold extraction waste liquor and precipitant solution, adjustment bio-oxidation flow velocity is 21m
3/ h, the precipitation agent flow velocity is about 11m
3/ h adjusts the flow velocity of precipitant solution at any time, pH=2.0 ± 0.2 in the control reactor, and 85 ℃ of temperature of reaction are carried out arsenic iron and are separated under the stirring intensity 700rpm/min condition;
2, adopt filtration or centrifugal separation technique, carry out solid-liquid separation, solid phase enters the tertiary iron phosphate preparation section, contains arsenic liquid and enters arsenic product preparation operation;
3, the washing of solid phase precipitation thing is 4 times, and aged at room temperature 11h behind the oven dry 7h, at air atmosphere, 600 ℃ of roasting 9h, obtains the tertiary iron phosphate product under air atmosphere, 100 ℃ of conditions of temperature;
4, gained contains arsenic liquid and enters the arsenic recovery process; To contain arsenic liquid, 1molL
-1Three kinds of liquid of the copper sulfate of concentration, ammoniacal liquor simultaneously and stream join in the reactor (b), containing arsenic liquid bare flow is 15m
3/ h contains arsenic liquid: the copper sulfate velocity ratio is controlled to be 10: 1, suitably adjusts the flow velocity of ammoniacal liquor, pH=4 ± 0.2 in the control reaction system, stirring intensity 400rpm/min carries out the cupric arsenate precipitin reaction, the liquid that flows out from reactor passes through solid-liquid separation, obtains the throw out of cupric arsenate;
5, the washing of cupric arsenate throw out is 4 times, aged at room temperature 4h, and after 4 hours, 400 ℃ of roasting 7h obtain the cupric arsenate product in 70 ℃ of oven dry of air atmosphere;
6, solution and the lime slurry of while after reactor (c) adds recovery arsenic, pH value of solution=8 ± 0.2 in the control still are under the condition of 700rpm/min at 60 ℃ of temperature, stirring intensity, obtain calcium sulphate solid by selective precipitation;
7, adopt filtration or centrifugal separation technique to realize solid-liquid separation, make building material product after the solid phase oven dry; Liquid returns the protista oxidation and puies forward the metal working preface behind the accent pH, realizes the whole process zero release.
Example 3
1, to handle 400m every day
3Bio-oxidation waste liquid (principal element Fe content is 45g/L, and As content is 8.5g/L) is an example.The recovery technological process of its valuable element is: Secondary ammonium phosphate is a precipitation agent, is made into 2molL
-1Ammonium dibasic phosphate solution, to reactor (a) in, add simultaneously acidic arsenic-containing biological oxidation gold extraction waste liquor and precipitant solution, adjustment bio-oxidation flow velocity is 21m
3/ h, the precipitation agent flow velocity is about 11m
3/ h adjusts the flow velocity of precipitant solution at any time, and with pH=2.5 ± 0.2 in the control reactor, 90 ℃ of temperature of reaction are carried out arsenic iron and separated under the stirring intensity 600rpm/min condition;
2, adopt filtration or centrifugal separation technique, carry out solid-liquid separation, solid phase enters the tertiary iron phosphate preparation section, contains arsenic liquid and enters arsenic product preparation operation;
3, the washing of solid phase precipitation thing is 5 times, aged at room temperature 10h, and behind the oven dry 7h, 120 ℃ of oven dry of air atmosphere 6h obtains the tertiary iron phosphate product under air atmosphere, 100 ℃ of conditions of temperature;
4, gained contains arsenic liquid and enters the arsenic recovery process; To contain arsenic liquid, 1molL
-1Three kinds of liquid of the copper sulfate of concentration, ammoniacal liquor simultaneously and stream join in the reactor (b), containing arsenic liquid bare flow is 25m
3/ h contains arsenic liquid: the copper sulfate velocity ratio is controlled to be 10: 1, suitably adjusts the flow velocity of ammoniacal liquor, pH=6 ± 0.2 in the control reaction system, stirring intensity 500rpm/min carries out the cupric arsenate precipitation, the liquid that flows out from reactor passes through solid-liquid separation, obtains the cupric arsenate throw out;
5, the washing of cupric arsenate throw out is 5 times, aged at room temperature 3h, and after 3 hours, 450 ℃ of roasting 6h obtain the cupric arsenate product in air atmosphere, 80 ℃ of oven dry;
6, solution and the lime slurry of while after reactor (c) adds recovery arsenic under pH value of solution value 9 ± 0.2 conditions, is under the condition of 600rpm/min at 40 ℃ of temperature, stirring intensity in the control still, obtains calcium sulphate solid by selective precipitation;
7, adopt filtration or centrifugal separation technique to realize solid-liquid separation, make building material product after the solid phase oven dry; Liquid returns the protista oxidation and puies forward the metal working preface behind the accent pH, realizes the whole process zero release.
Claims (7)
1. the precipitation agent (can be acid or salt) that in reactor (a), adds arsenic-containing biological oxidation gold extraction waste liquor and phosphorous acid group simultaneously, system pH is 1.5～2.5 in the control reactor, temperature of reaction is 75～90 ℃, at stirring intensity be under the condition of 600～800rpm/min by the selective precipitation tertiary iron phosphate, realize that arsenic iron separates.
2. adopt and filter or centrifugal separation technique realization solid-liquid separation, separate the preparation section that the back solid phase enters tertiary iron phosphate, liquid enters the preparation section of arsenic product.
The throw out tertiary iron phosphate through the washing 3-5 time after, aged at room temperature 10h～12h, after drying 6～8 hours under air atmosphere, 80～120 ℃ of conditions of temperature, roasting 8h～10h under 500～700 ℃ of conditions of temperature obtains the tertiary iron phosphate product.
4. add to reactor (b) in simultaneously through containing arsenic liquid and copper-bath after the solid-liquid separation, adopting ammoniacal liquor adjusting pH value 3～7, stirring intensity is 300～500rpm/min, obtains the cupric arsenate throw out by precipitin reaction.
5. the cupric arsenate throw out is after washing 3-5 time, aged at room temperature 2h～5h, and after air atmosphere, 60～80 ℃ were dried 3～5 hours, 350～450 ℃ of roasting 6h～8h obtained the cupric arsenate product.
6. simultaneously add solution and lime slurry after reclaiming arsenic to reactor (c), pH value of solution value 6～8 in the control still, 25 ℃～80 ℃ of temperature, stirring intensity are to obtain calcium sulfate precipitation by selective precipitation under the condition of 600～800rpm/min.
7. adopt and filter or centrifugal separation technique realization solid-liquid separation, make building material product after the oven dry of solid phase calcium sulfate after separating; Liquid returns the protista oxidation and puies forward the metal working preface, realizes the whole process zero release.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534187A (en) * | 2011-12-12 | 2012-07-04 | 师兆忠 | Method for treating pyrite cinder by combining acidic leaching with alkaline dissolving |
| CN114657375A (en) * | 2022-04-13 | 2022-06-24 | 东北大学 | Treatment method of arsenic-containing bacterial leachate |
| CN114835287A (en) * | 2022-04-15 | 2022-08-02 | 东北大学 | Method for circularly purifying metallurgical arsenic-containing acidic waste liquid and recycling sulfur |
| CN117512351A (en) * | 2024-01-04 | 2024-02-06 | 长春黄金研究院有限公司 | Process for separating and extracting valuable elements from biological oxidation liquid |
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| CN1103669A (en) * | 1993-12-07 | 1995-06-14 | 中国科学院化工冶金研究所 | Method of rocoverying gold silver and orpiment from refractory gold ore containing arsenic |
| WO2006087412A1 (en) * | 2005-02-16 | 2006-08-24 | Outotec Oyj. | Method for the recovery of gold from sulphide concentrate |
| CN101168450A (en) * | 2007-09-27 | 2008-04-30 | 中国黄金集团公司技术中心 | Method for separating and reclaiming arsenic and iron from acidic waste liquid containing arsenic acid and ferric sulfate |
| CN101168451A (en) * | 2006-10-25 | 2008-04-30 | 中南大学 | Method for preparing copper arsenite or copper arsenate by using arsenic-containing waste water |
-
2010
- 2010-03-10 CN CN2010101211942A patent/CN101805080B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103669A (en) * | 1993-12-07 | 1995-06-14 | 中国科学院化工冶金研究所 | Method of rocoverying gold silver and orpiment from refractory gold ore containing arsenic |
| WO2006087412A1 (en) * | 2005-02-16 | 2006-08-24 | Outotec Oyj. | Method for the recovery of gold from sulphide concentrate |
| CN101168451A (en) * | 2006-10-25 | 2008-04-30 | 中南大学 | Method for preparing copper arsenite or copper arsenate by using arsenic-containing waste water |
| CN101168450A (en) * | 2007-09-27 | 2008-04-30 | 中国黄金集团公司技术中心 | Method for separating and reclaiming arsenic and iron from acidic waste liquid containing arsenic acid and ferric sulfate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534187A (en) * | 2011-12-12 | 2012-07-04 | 师兆忠 | Method for treating pyrite cinder by combining acidic leaching with alkaline dissolving |
| CN114657375A (en) * | 2022-04-13 | 2022-06-24 | 东北大学 | Treatment method of arsenic-containing bacterial leachate |
| CN114835287A (en) * | 2022-04-15 | 2022-08-02 | 东北大学 | Method for circularly purifying metallurgical arsenic-containing acidic waste liquid and recycling sulfur |
| CN117512351A (en) * | 2024-01-04 | 2024-02-06 | 长春黄金研究院有限公司 | Process for separating and extracting valuable elements from biological oxidation liquid |
| CN117512351B (en) * | 2024-01-04 | 2024-04-12 | 长春黄金研究院有限公司 | Process for separating and extracting valuable elements from biological oxidation liquid |
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