CN103304062A - Method for treating lead-zinc sulfide ore production wastewater and recycling zinc from wastewater - Google Patents
Method for treating lead-zinc sulfide ore production wastewater and recycling zinc from wastewater Download PDFInfo
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- CN103304062A CN103304062A CN2013102718801A CN201310271880A CN103304062A CN 103304062 A CN103304062 A CN 103304062A CN 2013102718801 A CN2013102718801 A CN 2013102718801A CN 201310271880 A CN201310271880 A CN 201310271880A CN 103304062 A CN103304062 A CN 103304062A
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Abstract
The invention discloses a method for treating lead-zinc sulfide ore production wastewater and recycling zinc from wastewater. The method comprises the following steps of: 1) adding calcium carbonate ore into the lead-zinc sulfide ore production wastewater, stirring and reacting till the pH value of the wastewater is within 6.0-7.0, filtering, adding a flocculant into the obtained filtrate, stirring, standing, precipitating, and filtering so as to respectively obtain the de-ironed wastewater and ferric hydroxide slag; 2) adding sulfide and the flocculant into the de-ironed wastewater, stirring, standing, precipitating, and filtering so as to respectively obtain dezinced and de-ironed wastewater and zinc slag, wherein the sulfide is sodium sulfide or sodium bisulfide, and the sulfide is added in a solution manner; and 3) adding ferric hydroxide slag into the dezinced and de-ironed wastewater to react up, and filtering, wherein the filtrate can meet the discharge standard. The method is simple to operate, the discharge water treated by using the method can meet relevant national water discharge standard, and the recycling of heavy metal resource products and up-to-standard emission of wastewater are realized.
Description
Technical field
The present invention relates to the wastewater treating technology field, be specifically related to the method that zinc reclaims in the improvement of lead zinc sulphur ore factory effluent and the waste water.
Background technology
Mainly adopt at present the methods such as neutralization precipitation method, sulfide precipitation flotation process, ion exchange method, electrochemical process, biological process for the processing of nonferrous metal mine waste water, wherein, the neutralization precipitation method has the characteristics such as technique is simple, reliable, processing cost is low, it is the most frequently used method, the method mainly is by alkaline matters such as feeding lime or sodium hydroxide or yellow soda ash, improve the pH value of waste water, make the minimum oxyhydroxide of heavy metal ion formation solubility product in the waste water or carbonate deposition and remove.What the most often use in the existing neutralization precipitation method is lime neutralization and deriving method thereof, and the defective that these methods exist has: the pH value of (1) waste water is wayward; (2) valuable metal in the waste water can not reclaim as product; (3) produce the waste residue that contains in a large number various heavy, produce difficult treatment thereupon and may bring secondary heavy metal contamination.For concrete lead zinc sulphur ore, because the multi-component mineral of many metals of lead zinc sulphur ore are composed and are deposited characteristic, in the mining activity in production, factory effluent often is acid and contains the heavy metal contaminants such as a certain amount of Fe, Zn, Cd, if treated mining wastewater i.e. discharging not up to standard, except having the problems referred to above, regional surface water body is polluted, and make local ground watering body, farmland and ecotope be subject in various degree heavy metal contamination, and then by food chain serious harm HUMAN HEALTH.
Summary of the invention
The technical problem to be solved in the present invention provides the method that zinc reclaims in a kind of lead zinc sulphur ore factory effluent improvement and the waste water.The method is simple to operate, and is with low cost, adopts the waste water after the method is processed to be lower than the emission standard of national regulation, and can also obtain the Product-level zinc product that can sell when processing waste water, and economic benefit is higher.
The method that zinc reclaims in lead zinc sulphur ore factory effluent improvement of the present invention and the waste water may further comprise the steps:
1) add calcium carbonate mineral in the lead zinc sulphur ore factory effluent, stirring reaction to the pH value of waste water reaches between 6.0～7.0, filters, and adds flocculation agent in gained filtrate, stirs, and staticly settles, and filters, and obtains respectively except iron waste water and hydroxide scum;
2) in step 1) gained except adding sulfide and flocculation agent in the iron waste water, stir, staticly settle, filter, obtain respectively dezincifying except iron waste water and cadmia, this cadmia can directly be sold as zinc product;
Described sulfide is sodium sulphite or sodium bisulfide, and its form with the aqueous solution adds;
The add-on of described sulfide be the zine ion reaction in itself and the lead zinc sulphur ore factory effluent required stoichiometric 110～300%;
3) with step 1) the hydroxide scum of gained joins step 2) dezincification of gained reacts except in the iron waste water, filters, filtrate reaches emission standard, can be used as outer draining discharging.
The method of the invention is with the pH value conditioning agent of natural whiting ore as the lead zinc sulphur ore factory effluent, and remove iron ion in the waste water by the adjusting of pH value, because calcium carbonate mineral is originally as neutrality, hardly dissolving in water, has good pH damping characteristics after the reaction, thereby guarantee that the pH value effectively is controlled in 6.0～7.0 the scope, no matter and when the precipitated iron ion, add what natural whiting ore, can not cause waste water ph to surpass 7.0, this is because produce following reaction behind the adding natural whiting ore:
CaCO
3+H
+=Ca
2++OH
-+CO
2↑ （1）
Fe
3++3OH
-=Fe(OH)
3↓ （2）
Fe
2++2OH
-=Fe(OH)
2 （3）
4Fe(OH)
2+O
2+2H
2O→4Fe(OH)
3
Ca
2++SO
4 2+=CaSO
4 （4）
PH is lower, free H
+More, reaction (1) is faster; Near neutrality, free H
+Few, reaction is slow, (1) stopped reaction when neutrality; And along with the rising of pH value, react (2) reach 6.0～7.0 o'clock iron ion primitive reactions in the water to the pH value complete.
As seen can simply, effectively control the pH value of waste water by adding calcium carbonate stone, also solve simultaneously in the prior art interpolation lime or sodium hydroxide and caused the unmanageable problem of waste water ph.And in 6.0～7.0 pH value scope, the divalence in the waste water and ferric ion can precipitate fully, and the heavy metal ion such as zinc, cadmium then do not produce precipitation basically; The sulfide that adds afterwards is relatively stable in above-mentioned pH value scope, can with waste water in the heavy metal ion such as zine ion, cadmium ion fully react, generate metallic sulfide, become high-grade metal raw materials for metallurgy product; At last, the dezincification of having reclaimed heavy metal re-uses the hydroxide scum processing that the front operation produces except iron waste water, react except sulfide residual in the iron waste water by the iron in the hydroxide scum, zinc, lead, cadmium ion and dezincification, dezincify except unnecessary sulfide in the iron waste water to remove, after above-mentioned reaction, filtering, the filtrate of gained namely can be used as final discharge water, this final discharge water meets the standard (GB8978-1996) of the relevant discharge water of country, and wherein the content of the element such as each heavy metal well below above-mentioned standard; On the other hand, the heavy metal that is entrained in a small amount of waste water in the hydroxide scum reacts except sulfide residual in the iron waste water with dezincification, further stabilization, thus drop to the heavy metal secondary pollution that the hydroxide scum may cause minimum.
In the aforesaid method:
Step 1) in, total add-on of described calcium carbonate mineral is that the residue calcium carbonate mineral of the rear filtration gained that reacts completely recycles more than or equal to the required stoichiometry of the reaction of the hydrogen ion in itself and the lead zinc sulphur ore factory effluent.The required stoichiometry of acid-respons in described calcium carbonate mineral and the lead zinc sulphur ore factory effluent can calculate according to above-mentioned reaction formula (1), carry out fashionable dividing several times adding, also can once drop into excessive calcium carbonate mineral, not use if run out of separable out waiting until afterwards next time.Among the application, employed calcium carbonate mineral is generally CaCO
3The calcium carbonate mineral of content 〉=55.37% (quality), can certainly be other CaCO
3The calcium carbonate mineral of content.The granularity of described calcium carbonate mineral can be determined as required, if but its granularity is larger, the required reaction times can be a little longer, can react faster in order to make hydrogen ion and calcium carbonate mineral in the lead zinc sulphur ore factory effluent, and usually selecting granularity is the calcium carbonate mineral of 1～50mm; During calcium carbonate mineral in selecting above-mentioned size range, the hydrionic reaction times is about 0.5～24h in itself and the lead zinc sulphur ore factory effluent.
Step 1) and 2) in, described flocculation agent is selected poly-propionic acid amide (PAM) usually, its molecular weight (normally it is made into the aqueous solution use, the consumption of water gets final product for dissolving PAM) between 300～8,000,000.The consumption of flocculation agent is identical with existing conventional amount used, and particularly, its consumption can add 1～10 gram by waste water per ton and calculate.
Step 2) in, when sulfide was mixed with the aqueous solution, the consumption of water was the amount doesn't matter, but must dissolve the sulfide of institute's expense.In this step, sulfide is very fast with the reaction that removes iron waste water, just can finish most reaction at several minutes, therefore, described sulfide and flocculation agent can add simultaneously, add flocculation agent after also can adding first sulfide again, for guaranteeing to react completely, normally after adding sulfide 1～10min, add again flocculation agent, can certainly add again flocculation agent after the longer time at adding sulfide, but have little significance.
Step 2) medium sulphide content is as follows with the reaction formula that removes each metal in the iron waste water:
When sulfide is sodium sulphite:
Zn
+2+S
2-=ZnS↓
Cd
+2+S
2-=CdS↓
Pb
+2+S
2-=PbS↓
When sulfide is Sodium sulfhydrate:
Zn
2++HS
-=Zn S↓+H
-
Cd
2++HS
-=Cd S↓+H
-
Pb
2++HS
-=Pb S↓+H
-
HS when excessive
-+ H
-=H
2S ↑
Step 3) dezincification is as follows except the reaction formula of sulfide residual in the iron waste water and hydroxide scum in:
When sulfide is sodium sulphite:
Zn
+2+S
2-=ZnS↓
Cd
+2+S
2-=CdS↓
Pb
+2+S
2-=PbS↓
2Fe
3++3S
2-=Fe
2S
3↓
Fe
2++S
2-=Fe S↓
2S
2-+2O
2+H
2O=S
2O
3 2-+2OH
-
When sulfide is Sodium sulfhydrate:
Zn
2++HS
-=Zn S↓+H
-
Cd
2++HS
-=Cd S↓+H
-
Pb
2++HS
-=Pb S↓+H
-
Fe
2++S
2-=Fe S↓
2S
2-+2O
2+H
2O=S
2O
3 2-+2OH
-
Step 3) in, the time of reaction is about 10～60min.
In the technical scheme of the present invention, usually after adding flocculation agent, stir 1～10min, refilter after leaving standstill 5～60min.
The method of the invention especially is fit to Zn content greater than the improvement of the lead zinc sulphur ore factory effluent of 50mg/L.
Compared with prior art, the method for the invention has following characteristics:
1, with the natural whiting ore as regulating the waste water ph conditioning agent and with its precipitation agent as iron ion in the waste water, at first raw material sources are extensive, and are cheap, particularly more have superiority in south China karst area distributed more widely; Moreover add calcium carbonate stone can be simple, stable and effectively control the pH value of waste water, make precipitation of iron ions abundant, and be that good condition has been created in the recovery of the metal such as zinc;
2, use sulfide to reclaim except the heavy metal zinc in the iron waste water, cadmium etc., the content of Zn can directly as commodity selling, also can be sent into recovery process further refining in the cadmia that obtains more than 45% (quality);
3, reclaimed the dezincification of the heavy metals such as iron, zinc, cadmium except iron waste water, process with the hydroxide scum of precipitation again, react except sulfide residual in the iron waste water by ironic hydroxide and dezincification, dezincify except unnecessary sulfide in the iron waste water to remove, after above-mentioned reaction, filtering, the filtrate of gained namely can be used as final discharge water, and this final discharge water meets the standard of the relevant discharge water of country, and wherein the content of each element far below this standard; Realized that heavy metal produces the qualified discharge of resource product recovery and waste water;
4, the method for the invention is simple to operation, and is few to the pollution of environment, and has good economic benefit.
Embodiment
The invention will be further described with specific embodiment for the below, but the present invention is not limited to these embodiment.
Below among each embodiment related per-cent be mass percent.
Embodiment 1
1) getting plumbous zinc ore factory effluent 6L(wherein contains Zn837mg/L, contains Fe593mg/L, contains Cd4.15mg/L, pH value 2.8), place agitated pool, adding granularity is 3～5mm natural whiting ore (CaCO
3Content is 90%) 0.5kg, stir 1h, this moment, the pH value of waste water was 6.3, filtered, and the isolated natural whiting ore that has not reacted is waited until next time and used, (the PAM molecular weight is 3,000,000 to add concentration and be 1% the PAM aqueous solution in separating obtained filtrate, its solid consumption adds 5 grams by waste water per ton and calculates), stir 1min, form the ironic hydroxide flocculation sediment, filter, obtain respectively except iron waste water and hydroxide scum;
2) in step 1) gained except the Na that adds simultaneously 10% in the iron waste water
2S aqueous solution 150ml and concentration are that (the PAM molecular weight is 3,000,000 for 1% the flocculation PAM aqueous solution, its solid consumption adds 5 grams by waste water per ton and calculates), stir 1min, generate flocculation sediment, filter, obtain respectively dezincifying except iron waste water and filter residue, get 8.8g cadmia (zinc product) after the filter residue and drying, cadmia is analyzed, wherein each principal element content is: Zn55.78%, Cd0.27%, Pb＜0.01%;
3) in step 2) dezincification of gained is except adding step 1 in the iron waste water) the ironic hydroxide filter residue of gained, stirring reaction 50min filters, and gets oxidation scum 17.5g after the gained filter residue and drying, after measured, wherein the content of each principal element is: Fe20.24%, Pb＜0.01%, Cd＜0.01%; Gained filtrate namely can be used as the final outwards discharge water of discharging, and after measured, the content of each principal element is in this outer draining: Zn0.027mg/L, Cd＜0.001mg/L, Pb＜0.01mg/L, sulfide 0.6mg/L are lower than the relevant emission standard of country.
Embodiment 2
1) getting plumbous zinc ore factory effluent 40L(wherein contains Zn54mg/L, contains Fe136mg/L, contains Cd0.17mg/L, pH value 4.3), place steel basin and add 0.5～1.0mm calcium carbonate mineral (CaCO
3Content is 90%) 5kg, stir 5h, this moment, the pH value of waste water was 6.5, filtered, and the isolated natural whiting ore that has not reacted is waited until next time and used, adding concentration in separating obtained filtrate is that (the PAM molecular weight is 3,000,000 to the 1%PAM aqueous solution, its solid consumption adds 10 grams by waste water per ton and calculates), stir 3min, form the ironic hydroxide flocculation sediment, filter, obtain respectively except iron waste water and hydroxide scum;
2) in step 1) gained except the Na that adds 5% in the iron waste water
2S aqueous solution 150ml, adding concentration behind the 2min is that (the PAM molecular weight is 3,000,000 to the 1%PAM aqueous solution again, its solid consumption adds 2 grams by waste water per ton and calculates), stir 3min, generate flocculation sediment, filter, obtain respectively dezincifying except iron waste water and filter residue, after the filter residue and drying 3.9g cadmia (zinc product), cadmia is analyzed, wherein in each principal element content be: Zn53.59%, Cd0.17%, Pb＜0.01%;
3) in step 2) dezincification of gained is except adding step 1 in the iron waste water) the ironic hydroxide filter residue of gained, stirring reaction 1.5h filters, and gets oxidation scum 24.0g after the gained filter residue and drying, after measured, the content of each principal element is: Fe22.11%, Pb＜0.01%, Cd＜0.01%%; Gained filtrate namely can be used as the final outwards discharge water of discharging, and after measured, the content of each principal element is in this outer draining: Zn0.016mg/L, Cd＜0.001mg/L, Pb＜0.01mg/L, sulfide 0.7mg/L are lower than the relevant emission standard of country.
Embodiment 3
1) getting plumbous zinc ore factory effluent 1000L(wherein contains Zn688mg/L, contains Fe786mg/L, contains Cd3.62mg/L, pH value 2.6), place agitated pool and add 5～20mm calcium carbonate mineral (CaCO
3Content is 65%) 60kg, stir 15h, this moment, the pH value of waste water was 6.5, filtered, and the isolated natural whiting ore that has not reacted is waited until next time and used, adding concentration in separating obtained filtrate is that (the PAM molecular weight is 5,000,000 to the 1%PAM aqueous solution, its solid consumption adds 10 grams by waste water per ton and calculates), stir 10min, form the ironic hydroxide flocculation sediment, filter, obtain respectively except iron waste water and hydroxide scum;
2) in step 1) gained except the NaHS aqueous solution 4000ml that adds 15% in the iron waste water, (the PAM molecular weight is 5,000,000 to add concentration behind the 8min again and be 1% the PAM aqueous solution, its solid consumption adds 8 grams by waste water per ton and calculates), stir 15min, generate flocculation sediment, filter, obtain respectively dezincifying except iron waste water and filter residue, get 1245.5g cadmia (zinc product) after the filter residue and drying, cadmia is analyzed, each principal element content is wherein: Zn54.32%, Cd0.29%, Pb＜0.01%;
3) in step 2) dezincification of gained is except adding step 1 in the iron waste water) the ironic hydroxide filter residue of gained, stirring reaction 2h filters, and obtains oxidation scum 3688.0g after the gained filter residue and drying, after measured, wherein the content of each principal element is: Fe20.77%, Pb＜0.01%, Cd＜0.01%; Gained filtrate namely can be used as the final outwards discharge water of discharging, and after measured, the content of each principal element is in this outer draining: Zn0.02mg/L, Cd＜0.001mg/L, Pb＜0.01mg/L, sulfide 0.9mg/L are lower than the relevant emission standard of country.
Embodiment 4
1) getting plumbous zinc ore factory effluent 500L(wherein contains Zn54mg/L, contains Fe136mg/L, contains Cd0.17mg/L, pH value 4.3), place agitated pool and add 20～30mm calcium carbonate mineral (CaCO
3Content is 90%) 35kg, stir 20h, this moment, the pH value of waste water was 6.2, filtered, and the isolated natural whiting ore that has not reacted is waited until next time and used, (the PAM molecular weight is 8,000,000 to add concentration and be 1% the PAM aqueous solution in separating obtained filtrate, its solid consumption adds 1 gram by waste water per ton and calculates), stir 5min, form the ironic hydroxide flocculation sediment, filter, obtain respectively except iron waste water and hydroxide scum;
2) in step 1) gained except the Na that adds 20% in the iron waste water
2S aqueous solution 230ml, add again concentration behind the 5min and be 1% the PAM aqueous solution (the PAM molecular weight is 8,000,000, and its solid consumption adds 3 grams by waste water per ton and calculates), stir 10min, generate flocculation sediment, filter, obtain respectively dezincifying except iron waste water and filter residue, get 54.3g cadmia (zinc product) after the filter residue and drying, cadmia is analyzed, each principal element content is wherein: Zn48.58%, Cd0.15%, Pb＜0.01%;
3) in step 2) dezincification of gained is except adding step 1 in the iron waste water) the ironic hydroxide filter residue of gained, stirring reaction 5h filters, and obtains oxidation scum 311.0g after the gained filter residue and drying, after measured, wherein the content of each principal element is: Fe20.86%, Pb＜0.01%, Cd＜0.01%; Gained filtrate namely can be used as the final outwards discharge water of discharging, and after measured, the content of each principal element is in this outer draining: Zn0.06mg/L, Cd＜0.001mg/L, Pb＜0.01mg/L, sulfide 0.86mg/L are lower than the relevant emission standard of country.
Claims (5)
1. the method that zinc reclaims in the improvement of lead zinc sulphur ore factory effluent and the waste water is characterized in that may further comprise the steps:
1) add calcium carbonate mineral in the lead zinc sulphur ore factory effluent, stirring reaction to the pH value of waste water reaches between 6.0～7.0, filters, and adds flocculation agent in gained filtrate, stirs, and staticly settles, and filters, and obtains respectively except iron waste water and hydroxide scum;
2) in step 1) gained except adding sulfide and flocculation agent in the iron waste water, stir, staticly settle, filter, obtain respectively dezincifying except iron waste water and cadmia;
Described sulfide is sodium sulphite or sodium bisulfide, and its form with the aqueous solution adds;
The add-on of described sulfide be the zine ion reaction in itself and the lead zinc sulphur ore factory effluent required stoichiometric 110～300%;
3) with step 1) the hydroxide scum of gained joins step 2) dezincification of gained reacts except in the iron waste water, filters, filtrate namely reaches emission standard.
2. method according to claim 1, it is characterized in that: step 1) in, total add-on of described calcium carbonate mineral is that the filter residue calcium carbonate mineral of the rear filtration gained that reacts completely recycles more than or equal to the required stoichiometry of the reaction of the hydrogen ion in itself and the lead zinc sulphur ore factory effluent.
3. method according to claim 1 and 2 is characterized in that: step 1) in, the granularity of described calcium carbonate mineral is 1～50mm.
4. method according to claim 1 and 2 is characterized in that: step 1) and 2) in, described flocculation agent is poly-propionic acid amide.
5. method according to claim 1 and 2 is characterized in that: the consumption of flocculation agent adds 1～10 gram by waste water per ton and calculates.
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| CN104876369A (en) * | 2015-06-09 | 2015-09-02 | 长春黄金研究院 | Comprehensive treatment process of acid wastewater of nonferrous metal mine |
| CN107721007A (en) * | 2017-08-14 | 2018-02-23 | 内蒙古森泰企业咨询有限公司 | Lead-zinc sulfide ore mine wastewater step-by-step processing and sub-prime utilize technique |
| CN107964594A (en) * | 2016-10-20 | 2018-04-27 | 中冶节能环保有限责任公司 | A kind of method for reducing sintering heavy metals emission and recycling heavy metal |
| CN108751878A (en) * | 2018-08-22 | 2018-11-06 | 中国有色桂林矿产地质研究院有限公司 | A kind of curing agent and curing process of zinc abstraction waste residue |
| CN110551901A (en) * | 2019-10-18 | 2019-12-10 | 广西森合高新科技股份有限公司 | Method for recovering copper and lead from tail liquid and treatment method of leaching tail liquid generated by gold concentrate gold extraction process |
| CN111153521A (en) * | 2020-01-02 | 2020-05-15 | 湖南工程学院 | Method for removing lead and zinc ions in mine underground water under natural pH |
| CN111495581A (en) * | 2020-05-21 | 2020-08-07 | 广东省资源综合利用研究所 | Beneficiation method for recycling lead-zinc ore beneficiation treatment wastewater |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876369A (en) * | 2015-06-09 | 2015-09-02 | 长春黄金研究院 | Comprehensive treatment process of acid wastewater of nonferrous metal mine |
| CN107964594A (en) * | 2016-10-20 | 2018-04-27 | 中冶节能环保有限责任公司 | A kind of method for reducing sintering heavy metals emission and recycling heavy metal |
| CN107964594B (en) * | 2016-10-20 | 2019-05-10 | 中冶节能环保有限责任公司 | A method of reducing sintering heavy metals emission and recycling heavy metal |
| CN107721007A (en) * | 2017-08-14 | 2018-02-23 | 内蒙古森泰企业咨询有限公司 | Lead-zinc sulfide ore mine wastewater step-by-step processing and sub-prime utilize technique |
| CN108751878A (en) * | 2018-08-22 | 2018-11-06 | 中国有色桂林矿产地质研究院有限公司 | A kind of curing agent and curing process of zinc abstraction waste residue |
| CN108751878B (en) * | 2018-08-22 | 2021-08-03 | 中国有色桂林矿产地质研究院有限公司 | Curing agent and curing treatment process for zinc smelting waste residues |
| CN110551901A (en) * | 2019-10-18 | 2019-12-10 | 广西森合高新科技股份有限公司 | Method for recovering copper and lead from tail liquid and treatment method of leaching tail liquid generated by gold concentrate gold extraction process |
| CN110551901B (en) * | 2019-10-18 | 2021-05-18 | 广西森合高新科技股份有限公司 | Method for recovering copper and lead from tail liquid and treatment method of leaching tail liquid generated by gold concentrate gold extraction process |
| CN111153521A (en) * | 2020-01-02 | 2020-05-15 | 湖南工程学院 | Method for removing lead and zinc ions in mine underground water under natural pH |
| CN111495581A (en) * | 2020-05-21 | 2020-08-07 | 广东省资源综合利用研究所 | Beneficiation method for recycling lead-zinc ore beneficiation treatment wastewater |
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Application publication date: 20130918 |