CN103304052A - Treatment method of gold extraction cyaniding wastewater containing copper and iron ions with high concentration - Google Patents
Treatment method of gold extraction cyaniding wastewater containing copper and iron ions with high concentration Download PDFInfo
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Abstract
The invention discloses a treatment method of gold extraction cyaniding wastewater containing copper and iron ions with a high concentration. The treatment method comprises the steps of with zinc salt as a precipitator, removing a most part of free cyanogens and copper, iron and zinc ions in a solution, and further recovering residual cyanogens ions and other valuable metal ions in the solution after precipitation by using strong basic resin as an adsorbent to enable the wastewater to be discharged up to the standard. Due to the adoption of the treatment method, cyanide and the valuable metal ions in the gold extraction wastewater are furthest recovered by virtue of the two-step process of precipitation and resin adsorption; and moreover, as the treated wastewater can return to a leaching system or be directly discharged according to the needs, the treatment method is very strong in the flexibility, is low in treatment cost for treating the cyaniding wastewater with higher copper and iron contents and has a remarkable economic benefit.
Description
Technical field
The invention belongs to trade effluent comprehensive utilization technique field, particularly a kind of golden cyanide wastewater treatment process of putting forward of high density copper, iron ion that contains.
Background technology
Cyanide wastewater is the very strong trade effluent of a kind of toxicity, effluxes as not dealing carefully with directly, pollutes the environment, poisons biology, harm humans.The industry cyanide wastewater is mainly derived from the industries such as metallurgy, petrochemical industry, plating, organic synthesis, printing and dyeing, nitrogenous fertilizer and coal gas.The waste water complicated component, intractability is large.
The cyanide wastewater of solution of gold smelting plant is because the associated minerals in the Gold Ore remove all easy and prussiate generation copper cyanogen complex ions of chalcopyrite and chrysocolla and other copper mines.And mostly the implementation closed cycle system of smeltery is soaked gold, so when the immersion liquid of enriching Cu is returned gold mine and carried out Cyanide Leaching, cause the dual consumption of cyanogen.Bivalent cupric ion can nitrone ion, the cyanogen of generation volatilizees from solution, and univalent copper ion is combined meeting and is generated copper cyanogen complexing ion with free Cyanide, cause the very big consumption of prussiate to make leaching yield decline.
2Cu
2++ 8CN
-→ (CN)
2↑+2[Cu (CN)
3]
2-(formula 1)
Associated minerals pyrrhotite FeS and the white pyrite of gold mine have the hyperoxia voltinism, and in alkaline cyanide solution, meeting and prussiate and oxygen and alkali reaction generate a large amount of [Fe (CN)
6]
4-, react as follows:
FeS+3O
2+ 4CN
-+ 6H
2O → 4CNS
-+ 4Fe (OH)
3(formula 2)
FeS+6CN
-→ [Fe (CN)
6]
4-+ S
2-(formula 3)
FeS+2OH
-→ Fe (OH)
2+ S
2-(formula 4)
Fe (OH)
2+ 6CN
-→ [Fe (CN)
6]
4-+ 2OH
-(formula 5)
Iron cyano complex in the cyanide wastewater is very stable, when recycle, equally can continuous enrichment, and cause a large amount of consumption of leaching process cyanogen, make and soak golden Efficiency Decreasing.Simultaneously, when adopting ion exchange resin to carry out advanced treatment, affect the regeneration of resin, cause processing cost significantly to raise, the performance of enterprises descends.
So no matter the recycle of cyanide wastewater retrieval system, or qualified discharge after processing, what of these base-metal ion content all are the keys of considering.
The applicant finds present associated processing method and has problems as follows by retrieval:
The main method of Treatment of Cyanide-containing Wastewater has comprehensive absorption method and oxidative digestion method at present, but total development trend is tended to comprehensive absorption method.
The domestic method of ripe Treatment of Cyanide-containing Wastewater is acidization, in cyanide wastewater, add sulfuric acid, make the prussiate in the waste water be converted into low, the volatile HCN of boiling point, by the stripping effect, make HCN from liquid phase, use NaOH solution absorption, cycling and reutilization behind the stripping.But this method processing cost is high, and pH changes greatly, and the waste water after the processing is difficult to qualified discharge.
The ferrous sulfate method that document is mentioned is the yellow prussiate that prussiate is converted into iron, changes into Prussian blue type insoluble compound again, then filters out.But the water body that this method sludge is many, isolate behind the insolubles is blue; Processed waste water cyanogen residual quantity is 2-4mg/L, does not reach national standard, can not directly discharge, and should carry out advanced treatment in conjunction with other method.
Patent (CN101008090A) is mentioned with diaphragm electrodeposition and received the copper Treatment of Cyanide-containing Wastewater in conjunction with acidization, but equipment requirements is high, and is very high to the stability requirement of voltage, have the oxidation consumption situation of cyanogen to occur, and the metal that reclaims is more single.
Patent (CN102079590A) is mentioned with pure aluminum and phosphorus and being added in the cyanide wastewater, process high-concentration copper-containing waste water, but this method is introduced new pollutent phosphorus, and the reaction times is very long, and the pressure of stirring system is too large, and the metal of recovery is also more single.
Patent (CN1144194A) is mentioned a kind for the treatment of of waste water containing cyanogen by acidifying precipitation method, below sulfuric acid adjust pH to 3.5, precipitate each metal ion, add milk of lime and recall to alkalescence, prussic acid is processed through stripping repeatedly, but exists stripping equipment complicated, power consumption is large, sodium hydroxide consumption is large, and the waste water after processing still needs secondary treatment, can not directly discharge.
Patent (CN102491487A) is pointed out a kind of cyanide wastewater deep treatment method, to be oxygenant and anionite-exchange resin combination treatment cyanide wastewater with the chlorine that contains hypochlorite, but this method can only be processed the waste water of total cyanogen content 0.5-100mg/L, be not suitable for the processing of high cyanide containing wastewater, and the oxidation broken cyanide, prussiate can not recycle.
Patent (CN102452710A) and patent (CN102039128A) are pointed out a kind of Catalytic Wet Oxidation method of cyanide wastewater, and to be the catalyzer selected be at least a metal or its oxide compound in the elements such as supporting Pt, Pd, Ru, Ir, Rh on complex carrier to key.This catalyzer has improved the treatment effect of Catalytic Wet Oxidation method greatly, but the catalyzer cost of manufacture is high, is suitable for organic cyanide wastewater, and is bad to the removal effect of metal ion in the cyanide wastewater.
Patent (CN101875517A) points out that a kind of air that passes into is in the way of 14-16 hour oxide treatment cyanide wastewater of 130-150 ℃ of constant voltage reaction in reactor.Though without other assistant medicaments and material, but temperature is higher when processing, and the reaction times is very long, is not suitable for industrial applications.
Also have patent (CN102515388A) to point out the acid precipitation pre-treatment, use three sections alkaline chloride oxidation Treatment of Cyanide-containing Wastewater again, be fit to the processing of high cyanide containing wastewater, treatment effect is stable, but complex disposal process, and cyanide consumption is large, and processing cost is high.
Patent (CN1994934A) is pointed out the method for a kind of chemical precipitation-gamma-ray irradiation method Treatment of Cyanide-containing Wastewater, and this method is after zinc salt is precipitated prussiate, effluxes index thereby reach in conjunction with gamma-ray irradiation degraded prussiate again.But gamma-rays can destroy protein, nucleic acid and enzyme in the human body, causes the chemical process of human normal to be interfered, and serious can make necrocytosis.So this method has carcinogenic hidden danger to employee and peripheral personnel's health.
Patent (CN1141886A) is pointed out treatment of waste liquid containing cyanogen by ion exchange method, the copper iron zinc metal ion in the adsorbable waste liquid, but single ion exchange method, resin demand is large, processing cost is high, is not suitable for the processing of trade effluent in enormous quantities.
Patent (CN102311181A) patent proposes the method for a kind of embrane method and acidifying combined method Treatment of Cyanide-containing Wastewater, and this method is with embrane method useful component to be separated with unwanted component, and is simultaneously that unwanted component is concentrated, reclaims cyanogen after acid precipitation is processed.But this method exists film to clean difficult and the high characteristics of cost, and for large batch of wastewater treatment, equipment pressure is too large.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of golden cyanide wastewater treatment process of putting forward of high density copper, iron ion that contains, a large amount of valuable metals such as copper, iron, zinc and gold in can efficient recovery waste water, and treated waste water can return as required leaching system or directly efflux, and has very large handiness.
To achieve these goals, the technical solution used in the present invention is:
A kind of golden cyanide wastewater treatment process of carrying of high density copper, iron ion that contains, first take zinc salt as precipitation agent, most of free Cyanide and copper, iron, zine ion in the removal solution, utilize subsequently basic resin as sorbent material, further reclaim remaining cryanide ion and other valuable metal ions in the rear liquid of precipitation, so that discharged wastewater met the national standard.
The add-on of described precipitation agent must guarantee to precipitate that the content of free Cyanide and valuable metal ions satisfies the enterprise practical demand in the rear liquid, can directly return Leaching Systems recycles and is standard, as so that copper concentration is down to below the 2g/L, concentration of iron is down to below the 0.5mg/L.Concrete add-on can be calculated according to the content of Cu in waste water, and generally get its theoretical consumption 0.5～2.0 times, theoretical consumption calculates according to following formula: 2[Cu (CN)
2]
-+ Zn
2+=Zn (CN)
2↓+Cu
2(CN)
2↓.
Described zinc salt is zinc sulfate or zinc chloride and other soluble salt class materials, can solid form or be made into the aqueous solution and add.
The add-on volume ratio of described liquor capacity and sorbent material is (15～30): 1, and free Cyanide and other concentration of metal ions reach national industrial wastewater discharge primary standard in the assurance gold extraction waste water.
Described basic resin is 201 * 7 basic resins.
Know-why of the present invention is:
After zine ion adds cyanide wastewater, by adjusting its add-on, can with copper cyanogen, iron cyanogen and the zinc cyano complex is disposable to remove with precipitation forms, the correlated response formula is as follows:
2[Cu (CN)
2]
-+ Zn
2+=Zn (CN)
2↓+Cu
2(CN)
2↓ (formula 6)
Zn
2++ [Fe (CN)
6]
4-=Zn
2[Fe (CN)
6] ↓ (formula 7)
[Zn (CN)
4]
2-+ Zn
2+=2Zn (CN)
2↓ (formula 8)
Cyanide wastewater pH value after the processing is generally about 6～7, add later can directly the returning of an amount of sodium hydroxide and sodium cyanide and soak golden systemic circulation use, the waste water that need to efflux on a small quantity in addition can continue to adopt the absorption of 201 * 7 basic resins, recyclable valuable metal after the loaded resin desorb, resin returns adsorption system and recycles, discharged wastewater met the national standard.
Compared with prior art, advantage of the present invention is:
(1), this technology reclaimed prussiate and the valuable metal ions in the gold extraction waste water to greatest extent by precipitation and resin absorption two step process, and for copper, cyanide wastewater that iron level is higher, processing cost is low, remarkable in economical benefits.
(2), for the waste water that is necessary to return Leaching Systems, gold residual in the solution can remain in the solution, only needing to add a small amount of sodium cyanide and sodium hydroxide according to normal requirement just can satisfy fully and soak the lsp request index, reduce the add-on of sodium cyanide compared to acidization, greatly reduced enterprise cost.
(3), for the waste water that needs efflux, can adjust flexibly the consumption of precipitation agent, the binding resin adsorption deeply is processed again, thereby reaches the industrial wastewater discharge standard, but comprehensively recovering valuable metal again.
(4) but, also both combinations, most of waste water recycles after precipitation process, the sub-fraction waste water that surpasses the system capacity with the resin absorption advanced treatment after standard discharge, so also can reduce the workload of advanced treatment.
(5) precipitate the zinc sulfate saturated solution that after acid is molten, obtains and can be used as precipitation agent continuation use, saved again the consumption of precipitation agent.
As seen, this method has obvious economic benefit and environmental benefit.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
As shown in Figure 1, method of the present invention mainly is to add zinc salt such as zinc sulfate as precipitation agent in cyanide wastewater, most of free Cyanide and copper, iron, zine ion in the removal solution, solution part after the solid-liquid separation is returned leaching system, another part adds basic resin as sorbent material, adopt Adsorption and desorption technique, reclaim remaining cryanide ion and other valuable metal ions, so that discharged wastewater met the national standard.After throw out after the solid-liquid separation is used the dilute sulphuric acid acidleach, the zinc sulfate saturated solution that obtains is used for precipitation system, the prussic acid that volatilizes adopts liming or alkali liquor absorption to reclaim sodium cyanide, and throw out reclaims copper after roasting or other art breading.
According to above operational path, the invention provides specific embodiment as follows:
Embodiment one:
The cyanide wastewater of the present embodiment is taken from Henan solution of gold smelting plant 4# thickener, and waste water intermediate ion concentration determination result is as shown in table 1 before processing.
The metal ion content of table 1 stoste
| Species of metal ion in the waste water | CN -(mg/L) | Cu(g/L) | Fe(mg/L) | Zn(mg/L) | Au(mg/L) |
| Ionic concn (mg/L) | 760 | 4.5 | 62.9 | 249 | 0.34 |
Concrete operation step is as follows: respectively get 100ml waste water and be respectively charged in 6 200ml beakers, the zinc sulfate that adds different amounts stirs 1h, crosses leaching clear liquid measuring result as follows:
Table 2.ZnSO
4The experimental result that adds on-the-spot waste water
| The add-on of zinc sulfate (g/100ml) | 0.5 | 1.5 | 2.0 | 3.0 | 3.5 | 4.0 |
| Waste water residual copper amount (g/L) | 3.44 | 1.52 | 1.13 | 0.38 | 0.12 | 0.04 |
| Waste water residue gold amount (g/m3) | 0.34 | 0.33 | 0.38 | 0.37 | 0.35 | 0.34 |
As shown in Table 2, in the 100ml gold extraction waste water, add 2gZnSO
4, to stir after one hour, it is 1.13g/L that filtration obtains copper concentration residual in the supernatant liquor, simultaneously not loss of the gold in the waste water still remaines in the solution.Waste water after the processing can satisfy enterprise's production requirement, again add sodium cyanide and sodium hydroxide after, can directly return leaching system and recycle.
Consider to occur the saturated situation of the water yield in the actual production technique, therefore need regularly efflux a part of water.This part waste water is after the process precipitation process, continue to adopt 201 * 7 resins to adsorb, the waste water of using in this example adds the 5ml wet resin for adding the solution after 4g zinc sulfate is processed in every 100ml solution, normal temperature absorption 75min, the analytical results of liquid is as shown in table 3 after the absorption.
The concentration of each ion in the liquid after table 3. absorption
| Ionic species | CN-(mg/L) | Cu(mg/L) | Fe(mg/L) | Zn(mg/L) | Au(mg/L) |
| Ionic concn (mg/L) | 0.49 | 0.42 | 0 | 0.9 | 0 |
As shown in Table 3, free Cyanide and copper, iron, zinc ion concentration have all reached the emission standard of trade effluent in this part waste water, can directly efflux.
Loaded resin reclaims valuable metal after desorb, manipulation of regeneration, resin returns adsorption system and recycles;
Gained throw out diluted acid dissolving obtains returning precipitation workshop section behind the saturated solution of zinc sulfate, continues to use as precipitation agent, and the prussic acid of generation can return leaching system behind liming or alkali liquor absorption;
Throw out behind the dilute acid pretreatment can reclaim valuable metal through roasting or other technique.
Embodiment two:
The wastewater source of the present embodiment is in the waste water of certain solution of gold smelting plant, and the concentration of metal ions before the wastewater treatment is as shown in table 4.
The ion content of table 4 stoste
| Species of metal ion in the waste water | CN -(mg/L) | Cu(g/L) | Fe(mg/L) | Zn(mg/L) | Au(mg/L) |
| Ionic concn (mg/L) | 920 | 2.58 | 740 | 1180 | 0.31 |
Operation steps is as follows: respectively get 100ml waste water and be respectively charged in 6 200ml beakers, the zinc chloride that adds different amounts stirs 1h, crosses leaching clear liquid measuring result as follows:
Table 5. zinc chloride adds the experimental result of on-the-spot waste water
| The add-on of zinc chloride (g/100ml) | 1.0 | 1.5 | 2.0 | 2.5 | 3.0 | 4.0 |
| Waste water residual copper amount (g/L) | 1.98 | 1.32 | 0.75 | 0.36 | 0.17 | 0.021 |
| Waste water residue gold amount (g/m3) | 0.31 | 0.30 | 0.32 | 0.30 | 0.31 | 0.31 |
Known by table 5, add the 2.0g zinc chloride in the 100ml gold extraction waste water, the copper content after the precipitation in the liquid can reach 0.75g/L, and the content of useless underwater gold is unaffected, can satisfy need of production, again add sodium cyanide and sodium hydroxide after, can directly return leaching system and recycle.
Waste water is after the process precipitation process, can continue to adopt 201 * 7 resins to adsorb, the waste water of using in this example adds the 5ml wet resin for adding the solution after the 4g zinc chloride is processed in every 100ml solution, normal temperature absorption 75min, the analytical results of liquid is as shown in table 6 after the absorption.
The concentration of each ion in the liquid after table 6. absorption
| Ionic species | CN-(mg/L) | Cu(mg/L) | Fe(mg/L) | Zn(mg/L) | Au(mg/L) |
| Ionic concn (mg/L) | 0.45 | 0.34 | 0 | 1.2 | 0 |
As shown in Table 6, free Cyanide and copper, iron, zinc ion concentration have all reached the emission standard of trade effluent in the waste water, can directly efflux.
Among the above embodiment, used resin is 201 * 7 strong-basicity styrene series anion exchange resins that Chemical Plant of Nankai Univ. produces, and its performance perameter index is as follows:
1.pH scope: 1-14;
2. maximum operation (service) temperature: ℃ chlorine type≤80, hydrogen-oxygen type≤40 ℃;
Transition rate of expansion: (the 18-22% of Cl → OH);
4. industrial resin layer height: more than the 1.5m;
5. regenerated liquid concentration: NaOH:3-5%;
6. regenerated liquid consumption: volume: resin volume=3-5:1;
7. regenerated liquid flow velocity: 4-6m/h;
8. duration of contact: 45-60min regenerates;
9. positive wash is fast: 15-25m/h;
10. just wash the time: 30min;
11. operation flow velocity: 15-25m/h;
12. operating capacity: 〉=400mol/m.
Claims (5)
1. one kind contains the golden cyanide wastewater treatment process of putting forward of high density copper, iron ion, it is characterized in that: first take zinc salt as precipitation agent, most of free Cyanide and copper, iron, zine ion in the removal solution, utilize subsequently basic resin as sorbent material, reclaim remaining cryanide ion and other valuable metal ions in the rear liquid of precipitation, so that discharged wastewater met the national standard.
2. method of wastewater treatment according to claim 1 is characterized in that, the add-on of described precipitation agent is calculated according to the content of Cu in waste water, and get its theoretical consumption 0.5～2.0 times, theoretical consumption calculates according to following formula:
2[Cu(CN)
2]
-+Zn
2+=Zn(CN)
2↓+Cu
2(CN)
2↓。
3. method of wastewater treatment according to claim 1 is characterized in that, described zinc salt is zinc sulfate or zinc chloride, adds with solid form or aqueous solution.
4. method of wastewater treatment according to claim 1 is characterized in that, the add-on volume ratio of described liquor capacity and sorbent material is (15～30): 1.
5. according to claim 1 or 4 described method of wastewater treatment, it is characterized in that, described basic resin is 201 * 7 basic resins.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977029A (en) * | 2017-05-17 | 2017-07-25 | 哈工大新材料智能装备技术研究院（招远）有限公司 | A kind of cyaniding gold extraction waste water processing being combined based on soundization and cyclic utilization system |
| CN108840482A (en) * | 2018-05-31 | 2018-11-20 | 西安建筑科技大学 | A method of utilizing precipitating-electrolytic oxidation synergistic effect processing high-speed rail cyaniding gold extraction waste water |
| CN109127647A (en) * | 2018-07-17 | 2019-01-04 | 郑州经纬科技实业有限公司 | Cyanogen/fluoride method for innocent treatment in aluminium electrolytic tank |
| CN111101000A (en) * | 2019-12-27 | 2020-05-05 | 山东中城宏业矿业技术有限公司 | Device and method for removing zinc and iron in gold leaching barren solution of gold ore |
| CN111875024A (en) * | 2020-08-10 | 2020-11-03 | 紫金矿业集团股份有限公司 | Iron and cyanogen removing method for mixing copper-containing wastewater and cyanogen-containing wastewater |
| CN112863613A (en) * | 2021-01-25 | 2021-05-28 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining extreme value of dosage of copper salt for treating cyanide-containing wastewater by copper salt precipitation method |
| CN112863611A (en) * | 2021-01-14 | 2021-05-28 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining iron salt dosage extreme value in cyanide-containing wastewater treatment by iron salt precipitation method |
| CN115572026A (en) * | 2022-11-21 | 2023-01-06 | 山东齐鲁华信高科有限公司 | Method for treating waste liquid containing transition metal ion complex |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977029A (en) * | 2017-05-17 | 2017-07-25 | 哈工大新材料智能装备技术研究院（招远）有限公司 | A kind of cyaniding gold extraction waste water processing being combined based on soundization and cyclic utilization system |
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| CN108840482A (en) * | 2018-05-31 | 2018-11-20 | 西安建筑科技大学 | A method of utilizing precipitating-electrolytic oxidation synergistic effect processing high-speed rail cyaniding gold extraction waste water |
| CN109127647A (en) * | 2018-07-17 | 2019-01-04 | 郑州经纬科技实业有限公司 | Cyanogen/fluoride method for innocent treatment in aluminium electrolytic tank |
| CN111101000A (en) * | 2019-12-27 | 2020-05-05 | 山东中城宏业矿业技术有限公司 | Device and method for removing zinc and iron in gold leaching barren solution of gold ore |
| CN111875024A (en) * | 2020-08-10 | 2020-11-03 | 紫金矿业集团股份有限公司 | Iron and cyanogen removing method for mixing copper-containing wastewater and cyanogen-containing wastewater |
| CN112863611A (en) * | 2021-01-14 | 2021-05-28 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining iron salt dosage extreme value in cyanide-containing wastewater treatment by iron salt precipitation method |
| CN112863611B (en) * | 2021-01-14 | 2022-03-08 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining iron salt dosage extreme value in cyanide-containing wastewater treatment by iron salt precipitation method |
| CN112863613A (en) * | 2021-01-25 | 2021-05-28 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining extreme value of dosage of copper salt for treating cyanide-containing wastewater by copper salt precipitation method |
| CN112863613B (en) * | 2021-01-25 | 2022-07-29 | 山东黄金矿业科技有限公司选冶实验室分公司 | Method for determining extreme value of dosage of copper salt for treating cyanide-containing wastewater by copper salt precipitation method |
| CN115572026A (en) * | 2022-11-21 | 2023-01-06 | 山东齐鲁华信高科有限公司 | Method for treating waste liquid containing transition metal ion complex |
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