CN105648218A - Method for recovering zinc and iron from electroplating sludge with high iron content - Google Patents
Method for recovering zinc and iron from electroplating sludge with high iron content Download PDFInfo
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- CN105648218A CN105648218A CN201511027186.0A CN201511027186A CN105648218A CN 105648218 A CN105648218 A CN 105648218A CN 201511027186 A CN201511027186 A CN 201511027186A CN 105648218 A CN105648218 A CN 105648218A
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- Prior art keywords
- zinc
- iron
- electroplating sludge
- waste residue
- extraction
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recovering zinc and iron from electroplating sludge with high iron content. The method has the characteristics of low cost, high recovery rate and simple operation. The method comprises the following steps of: (a) leaching by using inorganic acid, to be specific, enabling the electroplating sludge to be in oscillatory reaction with hydrochloric acid at a room temperature, keeping still and then carrying out centrifugal separation to obtain leachate and waste residues; (b) removing chromium and iron by using a step-by-step precipitation method, to be specific, adding an alkaline solution to the leachate so as to adjust the pH value to 1-3, and removing Fe(OH)3 and Cr(OH)3 by filtering, thereby obtaining zinc-containing filtrate and waste residues; (c) recovering zinc by using an extraction method, to be specific, oscillating an extraction agent and the zinc-containing filtrate on a thermostatic water bath oscillator under the condition that the pH value is 1-3, and then keeping still for layering, thereby separating a water phase from an organic phase; (d) carrying out back extraction, to be specific, carrying out back extraction on zinc in the water phase by using sulfuric acid, and stabilizing the waste residues; and (e) stabilizing the waste residues generated in the steps (a) and (b) by using disodium hydrogen phosphate.
Description
Technical field
The present invention is specifically related to a kind of method reclaiming zinc and iron, more specifically relates to a kind of method reclaiming zinc and iron from high Fe content electroplating sludge.
Background technology
Electroplating wastewater processing process can produce the electroplating sludge containing the harmful heavy metals such as copper, nickel, zinc, chromium in a large number, this type of mud easily accumulates, easily run off, unstable, such as not treated any stacking, not only can cause serious secondary pollution, also can cause plurality of heavy metal resource loss.
The main processing ways of electroplating sludge is harmlessness disposing and recycling. Wherein harmlessness disposing comprises curing/stabilizing technology, fills out sea and stacking, thermochemical treatment technology etc.; Recycling comprises heavy metal recovery technology, material technology etc. (1) curing/stabilizing technology joins in electroplating sludge by solidifying agent, mix with mud, objectionable impurities in mud is not leached, thus decontamination, it it is an important technology disposing Hazardous wastes, there is the advantages such as cured body is stable, solidifying agent is easy to get, processing cost is low, it is a widely used Electroplating Sludge Technology at present. (2) the filling out sea disposal and can cause the pollution of ocean of electroplating sludge, stacking process electroplating sludge, not only needs a large amount of soil, and the place needing construction standard higher. Place election is improper, it is possible to body of groundwater can be made to pollute, the health of harmful to human. (3) the thermochemical treatment technology of electroplating sludge refers to and decomposes electroplating sludge under the high temperature conditions, reduce the toxicity of mud, make mud volume reduction fast, and make full use of valuable material in mud, its advantage be reduction of in electroplating sludge severe toxicity composition toxicity, the quick volume reduction of mud can be made, and make full use of valuable material in mud; But shortcoming needs energy consumption height, need to invest and working cost height. (4) in electroplating sludge, the research focus of heavy metal recovery is hydrometallurgic recovery, comprises chemical precipitation method, solvent extration, reduction method, electrodip process, microbial method etc. (5) material technology disposal electroplating sludge refers to and is applied in the production process of material of construction or other materials as raw material or auxiliary material by electroplating sludge. Research shows, it is feasible that material technology disposes electroplating sludge, but there is the problem such as less economical of secondary pollution and products obtained therefrom.
It is thus desirable to research and develop a kind of method that technique simply and not produces secondary pollution to solve prior art Problems existing.
Summary of the invention
It is an object of the invention to solve prior art Problems existing with not enough, a kind of method reclaiming zinc and iron from high Fe content electroplating sludge is provided, the method is the recovery method proposed for high Fe content electroplating sludge, has that cost is low, rate of recovery height, feature simple to operate.
The present invention is achieved by the following technical solutions:
The method reclaiming zinc and iron from high Fe content electroplating sludge of the present invention, it comprises the following steps:
A () mineral acid leaches: at room temperature, by electroplating sludge and hydrochloric acid oscillatory reaction, and after leaving standstill, centrifugation obtains leach liquor and waste residue;
B () step-by-step precipitation method removes chromium, iron: add alkaline solution adjust ph in leach liquor to 1-3, can remove Fe (OH) after filtration3With Cr (OH)3, and obtain containing zinc filtrate and waste residue;
C () extraction process reclaims zinc: when pH value is 1-3, vibrate afterwards stratification by extraction agent with containing zinc filtrate, be separated with organic phase by aqueous phase on water bath with thermostatic control vibrator;
D () is stripped: zinc of being stripped by aqueous phase sulfuric acid;
(e) waste residue stabilization: step (a) and the middle waste residue produced of step (b) use Sodium phosphate dibasic to carry out stabilization.
The above-mentioned method of the present invention, its further technical scheme is the concentration of hydrochloric acid described in step (a) is 2-5mol/L, and the reaction times is 1-4h.
The above-mentioned method of the present invention, its further technical scheme can also be the alkaline solution described in step (b) is NaOH solution, and concentration is 5-8mol/L.
The above-mentioned method of the present invention, the sulfonated kerosene solution of its further technical scheme can also to be the extraction agent described in step (c) be 2-ethylhexyl phosphoric acid list (2-ethylhexyl) ester, volume percent is 25%-35%, and it is 1-2 that O/A scope is compared in control.
The above-mentioned method of the present invention, its further technical scheme can also be the sulfuric acid concentration described in step (d) is 1-5mol/L, and comparing O/A scope is 1-2, back-extraction time 5-10min.
The above-mentioned method of the present invention, its further technical scheme can also be the addition of the Sodium phosphate dibasic described in step (e) is the 15%-30% of waste residue weight.
Wherein compare the volume ratio that O/A refers to organic phase and aqueous phase.
The present invention compared with prior art, has the following advantages and effect:
1, the research utilized by the electric plating sludge resource that iron level is lower at present is more, and the research of the electroplating sludge of high Fe content is less, the present invention is directed to the recovery process that high Fe content electroplating sludge proposes and have that cost is low, rate of recovery height, advantage simple to operate.
2, mineral acid (hydrochloric acid) is to the leaching yield of zinc up to more than 70%, is about 60% to the leaching yield of iron. Mineral acid leaching and fractional precipitation are removed the metals such as iron and are all ripe method efficiently, it is intended to further high efficiente callback zinc.
3, the waste residue that electroplating sludge and recovery heavy metal process produce is carried out stabilization treatment research by the present invention simultaneously; it is intended to make it environmental sound; thus realizing the minimizing of electroplating sludge, resource utilization and innoxious, protection of the environment, brings economy, society and environmental benefit.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the method reclaiming zinc and iron from high Fe content electroplating sludge of the present invention.
Embodiment
Table 1 is the content of each heavy metal in electroplating sludge.
Heavy metal content in table 1 electroplating sludge
Embodiment 1
As shown in Figure 1, the concrete operation steps of the present invention has: mineral acid leaches, iron is removed in fractional precipitation and chromium, extraction process reclaim zinc, reextraction and waste residue stabilization.
(1) mineral acid leaches: the hydrochloric acid adding 3mol/L in dry mud, under 20 DEG C of conditions, is placed in water-bath constant temperature oscillator vibration (200r/min) 1h, leaves standstill the centrifugal 7min of 30min, 4000r/min.
(2) step-by-step precipitation method removes chromium, iron: add 5mol/LNaOH adjust ph to 1 in electroplating sludge leach liquor, stirs precipitin reaction 2h, can remove Fe (OH) after filtration3With Cr (OH)3��
(3) extraction process reclaims zinc: choose P507 (2-ethylhexyl phosphoric acid list (2-ethylhexyl) ester) as extraction agent, sulfonated kerosene is as thinner, when pH value is 2, add volumetric concentration be 30% P507 and containing zinc filtrate, compare O/A=1, vibrate 8min on water bath with thermostatic control vibrator, is placed in separating funnel stratification, is separated with organic phase by aqueous phase.
(4) strip: stripping zinc with sulfuric acid, sulfuric acid concentration is 1mol/L, compares O/A=1, back-extraction time 6min.
(5) waste residue stabilization: the waste residue that mineral acid leaches generation in the process removing chromium, iron with fractional precipitation uses Sodium phosphate dibasic to carry out stabilization. Sodium phosphate dibasic and waste residue are fully mixed, Sodium phosphate dibasic addition is 15%, indoor place 7d continuously, every day stirs once, the precipitation being 4.5,7,10 by pH value carries out leaching experiment, copper, nickel, zinc, chromium leach concentration and reach leaching characteristic identification standard value in " Hazardous wastes judging standard leaching characteristic identification " (GB5085.3-2007), and now electroplating sludge stabilization effect is good.
Concentration of heavy metal ion in table 2 waste residue leach liquor
Embodiment 2
(1) mineral acid leaches: the hydrochloric acid adding 2mol/L in dry mud, under 20 DEG C of conditions, is placed in water-bath constant temperature oscillator vibration (200r/min) 1h, leaves standstill the centrifugal 7min of 30min, 4000r/min.
(2) step-by-step precipitation method removes chromium, iron: add 5mol/LNaOH adjust ph to 2 in electroplating sludge leach liquor, stirs precipitin reaction 2h, can remove Fe (OH) after filtration3With Cr (OH)3��
(3) extraction process reclaims zinc: choose P507 (2-ethylhexyl phosphoric acid list (2-ethylhexyl) ester) as extraction agent, sulfonated kerosene is as thinner, when pH value is 2, add volumetric concentration be 25% P507 and containing zinc filtrate, compare O/A=1, vibrate 8min on water bath with thermostatic control vibrator, is placed in separating funnel stratification, is separated with organic phase by aqueous phase.
(4) strip: stripping zinc with sulfuric acid, sulfuric acid concentration is 1mol/L, compares O/A=1, back-extraction time 5min.
(5) waste residue stabilization: the waste residue that mineral acid leaches generation in the process removing chromium, iron with fractional precipitation uses Sodium phosphate dibasic to carry out stabilization. Sodium phosphate dibasic and waste residue are fully mixed, Sodium phosphate dibasic addition is 15%, indoor place 7d continuously, every day stirs once, the precipitation being 4.5,7,10 by pH value carries out leaching experiment, copper, nickel, zinc, chromium leach concentration and reach leaching characteristic identification standard value in " Hazardous wastes judging standard leaching characteristic identification " (GB5085.3-2007), and now electroplating sludge stabilization effect is good.
Concentration of heavy metal ion in table 3 waste residue leach liquor
Embodiment 3
(1) mineral acid leaches: the hydrochloric acid adding 5mol/L in dry mud, under 20 DEG C of conditions, is placed in water-bath constant temperature oscillator vibration (200r/min) 4h, leaves standstill the centrifugal 7min of 30min, 4000r/min.
(2) step-by-step precipitation method removes chromium, iron: add 5mol/LNaOH adjust ph to 3 in electroplating sludge leach liquor, stirs precipitin reaction 2h, can remove Fe (OH) after filtration3With Cr (OH)3��
(3) extraction process reclaims zinc: choose P507 (2-ethylhexyl phosphoric acid list (2-ethylhexyl) ester) as extraction agent, sulfonated kerosene is as thinner, when pH value is 2, add volumetric concentration be 35% P507 and containing zinc filtrate, compare O/A=2, vibrate 8min on water bath with thermostatic control vibrator, is placed in separating funnel stratification, is separated with organic phase by aqueous phase.
(4) strip: stripping zinc with sulfuric acid, sulfuric acid concentration is 5mol/L, compares O/A=2, back-extraction time 10min.
(5) waste residue stabilization: the waste residue that mineral acid leaches generation in the process removing chromium, iron with fractional precipitation uses Sodium phosphate dibasic to carry out stabilization. Sodium phosphate dibasic and waste residue are fully mixed, Sodium phosphate dibasic addition is 30%, indoor place 7d continuously, every day stirs once, the precipitation being 4.5,7,10 by pH value carries out leaching experiment, copper, nickel, zinc, chromium leach concentration and reach leaching characteristic identification standard value in " Hazardous wastes judging standard leaching characteristic identification " (GB5085.3-2007), and now electroplating sludge stabilization effect is good.
Concentration of heavy metal ion in table 4 waste residue leach liquor
Claims (6)
1. one kind is reclaimed the method for zinc and iron from high Fe content electroplating sludge, it is characterised in that comprise the following steps:
A () mineral acid leaches: at room temperature, by electroplating sludge and hydrochloric acid oscillatory reaction, and after leaving standstill, centrifugation obtains leach liquor and waste residue;
B () step-by-step precipitation method removes chromium, iron: add alkaline solution adjust ph in leach liquor to 1-3, can remove Fe (OH) after filtration3With Cr (OH)3, and obtain containing zinc filtrate and waste residue;
C () extraction process reclaims zinc: when pH value is 1-3, vibrate afterwards stratification by extraction agent with containing zinc filtrate, be separated with organic phase by aqueous phase on water bath with thermostatic control vibrator;
D () is stripped: zinc of being stripped by aqueous phase sulfuric acid;
(e) waste residue stabilization: step (a) and the middle waste residue produced of step (b) use Sodium phosphate dibasic to carry out stabilization.
2. method according to claim 1, it is characterised in that the concentration of hydrochloric acid described in step (a) is 2-5mol/L, the reaction times is 1-4h.
3. method according to claim 1, it is characterised in that the alkaline solution described in step (b) is NaOH solution, concentration is 5-8mol/L.
4. method according to claim 1, it is characterized in that the extraction agent described in step (c) is the sulfonated kerosene solution of 2-ethylhexyl phosphoric acid list (2-ethylhexyl) ester, volume percent is 25%-35%, and it is 1-2 that O/A scope is compared in control.
5. method according to claim 1, it is characterised in that the sulfuric acid concentration described in step (d) is 1-5mol/L, comparing O/A scope is 1-2, back-extraction time 5-10min.
6. method according to claim 1, it is characterised in that the addition of the Sodium phosphate dibasic described in step (e) is the 15%-30% of waste residue weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511027186.0A CN105648218A (en) | 2015-12-31 | 2015-12-31 | Method for recovering zinc and iron from electroplating sludge with high iron content |
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| CN201511027186.0A CN105648218A (en) | 2015-12-31 | 2015-12-31 | Method for recovering zinc and iron from electroplating sludge with high iron content |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107299219A (en) * | 2017-06-27 | 2017-10-27 | 郑州中科新兴产业技术研究院 | A kind of resource utilization method of electroplating sludge |
| CN108570557A (en) * | 2017-03-14 | 2018-09-25 | 湖南埃格环保科技有限公司 | The separation method of iron, chromium, nickel, copper, zinc in a kind of high chromium electroplating sludge leachate of high ferro |
| CN108754150A (en) * | 2018-06-24 | 2018-11-06 | 江西理工大学 | A kind of method of valuable metal in electroplated mud synthetical recovery |
| CN110484730A (en) * | 2019-08-14 | 2019-11-22 | 广州科城环保科技有限公司 | A method of recycling feed grade basic zinc chloride from zinc-containing sludge |
| CN113862482A (en) * | 2021-10-08 | 2021-12-31 | 上海良仁化工有限公司 | Process for recovering chromium, copper, nickel and cobalt from electroplating sludge |
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| JP2012102350A (en) * | 2010-11-08 | 2012-05-31 | Sumitomo Metal Mining Co Ltd | Method for recovering valuable metal |
| CN104178642A (en) * | 2014-08-31 | 2014-12-03 | 中南大学 | Method for separating zinc and iron from zinc leaching residues |
| CN104593598A (en) * | 2014-12-18 | 2015-05-06 | 北京矿冶研究总院 | Method for resource utilization of multiple metals in electroplating sludge |
| CN105200239A (en) * | 2015-09-29 | 2015-12-30 | 广西银亿再生资源有限公司 | Method of separating and recovering zinc from electroplating sludge |
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2015
- 2015-12-31 CN CN201511027186.0A patent/CN105648218A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012102350A (en) * | 2010-11-08 | 2012-05-31 | Sumitomo Metal Mining Co Ltd | Method for recovering valuable metal |
| CN104178642A (en) * | 2014-08-31 | 2014-12-03 | 中南大学 | Method for separating zinc and iron from zinc leaching residues |
| CN104593598A (en) * | 2014-12-18 | 2015-05-06 | 北京矿冶研究总院 | Method for resource utilization of multiple metals in electroplating sludge |
| CN105200239A (en) * | 2015-09-29 | 2015-12-30 | 广西银亿再生资源有限公司 | Method of separating and recovering zinc from electroplating sludge |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108570557A (en) * | 2017-03-14 | 2018-09-25 | 湖南埃格环保科技有限公司 | The separation method of iron, chromium, nickel, copper, zinc in a kind of high chromium electroplating sludge leachate of high ferro |
| CN107299219A (en) * | 2017-06-27 | 2017-10-27 | 郑州中科新兴产业技术研究院 | A kind of resource utilization method of electroplating sludge |
| CN107299219B (en) * | 2017-06-27 | 2019-02-22 | 郑州中科新兴产业技术研究院 | A kind of resource utilization method of electroplating sludge |
| CN108754150A (en) * | 2018-06-24 | 2018-11-06 | 江西理工大学 | A kind of method of valuable metal in electroplated mud synthetical recovery |
| CN110484730A (en) * | 2019-08-14 | 2019-11-22 | 广州科城环保科技有限公司 | A method of recycling feed grade basic zinc chloride from zinc-containing sludge |
| CN113862482A (en) * | 2021-10-08 | 2021-12-31 | 上海良仁化工有限公司 | Process for recovering chromium, copper, nickel and cobalt from electroplating sludge |
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Application publication date: 20160608 |