CN102173547B - Resource recycling process for nickel-containing sludge in electroplating enterprises - Google Patents
Resource recycling process for nickel-containing sludge in electroplating enterprises Download PDFInfo
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Abstract
The invention relates to a resource recycling process for nickel-containing sludge in electroplating enterprises. In the process, the nickel-containing sludge generated in the electroplating enterprises is used as a treatment target, and nickel in the sludge is subjected to resource recycling treatment by a calcining, acid leaching, impurity removing and alkaline precipitating combined method. The process comprises the following steps of: calcining and purifying the nickel-containing sludge to remove moisture and organic matters from the sludge; crushing calcined residues, and leaching by using sulfuric acid solution; electrolyzing leaching liquid to remove copper, and removing ferrum, calcium and magnesium impurities by a chemical precipitation method; and alkalifying to obtain nickel hydroxide precipitates so as to recover the nickel in the sludge. In the resource recycling process, the removal rate of the impurities is more than 99 percent, the recovery rate of the nickel is more than 96 percent, the pollution of the sludge to environment is reduced, the value of the sludge is realized, and environmental and economic benefits are obvious.
Description
Technical field
The present invention relates to the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise, the combined method of particularly a kind of roasting, sulfuric acid leaching, removal of impurities and alkaline chemical precipitation is handled the technology of the nickeliferous mud of electroplating enterprise generation.
Background technology
Electroplating industry is the important processing industry of China; Extensively be distributed in the every profession and trade, but different plating and products must select for use each heavy metal species such as gold, silver, copper, nickel, chromium, zinc, iron, cadmium etc. as raw material in a large number; In electroplating process, the part heavy metal can get in the waste water.According to incompletely statistics, the electroplating wastewater generation of China is about 4,000,000,000 m
3/ year, be equivalent to the water service amount of several big and medium-sized cities, be one of pollution industry of emphasis.Electroplating sludge is the emission that produces in the electroplating wastewater processing process, is a kind of typical hazardous waste, and the heavy metal that is present in wherein infiltrates in soil and the water easily, severe contamination surface water and underground water, and the harm surrounding enviroment, healthy until harm humans.
The nickeliferous mud of electroplating enterprise mainly is that the plating nickel-containing waste water that produces in the electroplating enterprise nickel plating technology process is handled the mud that the back forms.The mud of this technical study is the nickeliferous mud of non-chromium electroplating enterprise; Wherein the content of nickel generally about 5%, reaches as high as 10%, and the content of copper, iron is about 1%; Owing in the electroplating wastewater processing process, adopt lime; Therefore, may bring calcium, magnesium addition in the mud, moisture percentage in sewage sludge is about 70～75%.Because nickel content is lower, adds that impurity is more, reclaiming has certain difficulty, generally takes modes such as security landfill, burning to dispose.Should pay bigger processing cost like this, waste nickel resources again.Therefore, the nickeliferous mud of secondary recycling resource of this cheapness is carried out economy, resource recycling efficiently, realize turning waste into wealth, not only can eliminate environmental pollution, can also produce favorable economic benefit.
At present, because China's electroplating industry exists that factory point is many, small scale, equipment are hanged down and reached problems such as the pollution control level is low, most of electroplating sludge does not all obtain disposal effectively and reasonably, and environment has been caused serious pollution.Therefore, how to take otherwise effective technique treatment and disposal electroplating sludge, and realize its stabilisation, innoxious and resource, always be the domestic and international research emphasis.The domestic and international at present resource recovery technology to metal in the electroplating sludge mainly contains chemical precipitation method, solvent extraction, ion-exchange etc.Because valuable metal content is lower in the electroplating sludge, the mud medium is complicated, and, complex process big to the recycling equipment investment of valuable metal, operation cost are high, so that the resource of electroplating sludge is recycled and failed to form ripe production model always.
Summary of the invention
The present invention provides the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise, and purpose is that resource, problem of environment pollution caused recycled, wasted to the nickeliferous mud that solves the electroplating enterprise generation can not resource.
For achieving the above object, the technical scheme that the present invention adopts is: the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise, mainly form by the following step:
The first step: roasting purifying
With the quality percentage composition of moisture is 70～75% nickeliferous mud, and roasting obtained the roasting residue in 5～6 hours under 600～700 ℃ of conditions;
Second step: sulfuric acid leaches
Add water after the roasting residue that at first first step is obtained is pulverized and mix and make mud, under stirring condition, in said mud, add sulfuric acid then, make nickel element and sulfuric acid in the said mud fully react the generation nickelous sulfate, obtain sulphuric leachate; Wherein, said sulfuric acid with roasting residue mixed proportion between the two is: per 2～3 milliliters of sulfuric acid mix with 1 gram roasting residue; The concentration of said sulfuric acid is 3～4mol/l;
The 3rd step: filter
With the sulphuric leachate cooling that second step obtained, filter then and obtain filtrating and filter residue;
The 4th step: electrolysis copper removal
Obtaining electrolyte below regulating the 3rd pH value of filtrate to 1 or 1 that obtain of step, is the said electrolyte of electrolysis under 2～2.5 volts the condition at voltage then, and the concentration of copper ion in this electrolyte is reduced to below the 5mg/l, obtains the surplus liquid of electrolysis;
The 5th step: iron impurity
In the 4th surplus liquid of electrolysis that obtains of step, add sodium chlorate; Make the abundant oxidation of ferrous ion in the surplus liquid of said electrolysis generate ferric ion; Then under 80～90 ℃ of conditions; The pH value is transferred to 3.9～4.1, make said ferric ion generate ferric hydroxide precipitate fully, obtain deironing filtrating after the filtration;
The 6th step: removing calcium and magnesium impurity
The deironing pH value of filtrate that the 5th step was obtained transfers to 4.5～6, under 80～90 ℃ of conditions, adds sodium fluoride then, makes calcium ion and magnesium ion in the said deironing filtrating generate calcirm-fluoride and magnesium fluoride deposition respectively, obtains removing calcium and magnesium filtrating after the filtration; Wherein, add 1～10g sodium fluoride in every liter of deironing filtrating;
The 7th step: alkaline chemical precipitation
Under stirring condition; Adding quality percentage composition was 25～35% sodium hydrate aqueous solution during the removing calcium and magnesium that obtains to the 6th step was filtrated; Make that said removing calcium and magnesium pH value of filtrate is 9～10; Make the nickel ion in the said removing calcium and magnesium filtrating generate nickel hydroxide precipitate, the filter cake that obtains after the filtration is nickel hydroxide.
Related content in the technique scheme is explained as follows:
1, in the such scheme, residue washing to the neutrality that said the 3rd step is obtained obtains cleaning solution, and this cleaning solution can be back to the preparation that is used to leach reagent of sulfuric acid in second step.
2, in the such scheme, in said the 5th step, the pH value is transferred to 3.5～4.0 with the aqueous sodium carbonate of 80～100g/l.
3, in the such scheme, in said the 6th step, using the quality percentage composition is that 25～35% sodium hydrate aqueous solution transfers to 4.5～6 with the pH value.
Because the technique scheme utilization, the present invention compared with prior art has advantage and effect:
1, the present invention at first carries out roasting to nickeliferous mud, and moisture and organic matter can burn mistake after the roasting, and moisture can be burnt basically fully, burns the organic components of losing and accounts for about 30% of mud butt weight.Nickeliferous mud can effectively reduce moisture and organic matter in the mud through after the roasting, has realized the minimizing of mud, has reduced the medicament use amount that subsequent recovery is handled, and produce heat because organic matter self burns in this process, so energy consumption is low.
2, removal of impurity of the present invention reaches more than 99%, and nickel recovery can reach more than 96%, has not only reduced the pollution of mud to environment, has also realized value, environment and the remarkable in economical benefits of mud.
Description of drawings
Accompanying drawing 1 is flow chart of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Embodiment one: the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise
Shown in accompanying drawing 1, the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise, concrete steps are following:
(1) roasting purifying
Nickeliferous mud moisture content after press filtration also contains the organic matters composition in the mud simultaneously 73%.With mud roasting in roaster, the control sintering temperature is 600～700 ℃, and roasting time is 6 hours, and moisture and organic matter can burn mistake after the roasting, and moisture can be burnt basically fully, burns the organic components of losing and accounts for about 30% of mud butt weight.Mud can effectively reduce moisture and organic matter in the mud through after the roasting, has realized the minimizing of mud, has reduced the medicament use amount that subsequent recovery is handled, and this process energy consumption is lower.
(2) sulfuric acid leaches
It is most widely used a kind of method in the solid waste lixiviation process that acidleach goes out, and specifically adopting which kind of acid to leach needs to decide according to the character of solid waste.In the processing of industrial wastes such as plating, casting, smelting, sulfuric acid is a kind of reagent that comparatively effectively leaches.Have characteristics such as low price, little, the difficult decomposition of volatility is widely used owing to it.Research shows that sulfuric acid can reach 95%～100% to the leaching rate of copper, nickel in the electroplating enterprise wastewater treatment mud.The many forms with hydroxide of metallic element in the electroplating sludge exist, and mud is after roasting, and part hydroxide can resolve into oxide, Ni
2+, Cu
2+, Fe
2+The pH value of hydrolytic precipitation is respectively 6.7,5.1,6.1, and the pH value of hydrolytic precipitation is high more, under with the situation of acidity, just leaches more easily, and acidity is high more, and metal leaching rate is just high more.
Get the residue after an amount of roasting, after pulverizing, add low amounts of water and stir pulp, with liquid-solid ratio (liquid volume and solid masses ratio) 2: 1, slowly add the sulfuric acid of 3.5mol/l, stirring reaction is 2 hours at normal temperatures.Carry out suction filtration after the cooling, measure the concentration of nickel in the leachate, the leaching rate of nickel reaches 99%.To neutral, cleaning solution returns and is used to prepare sulfuric acid leached mud with the low amounts of water washing, and leached mud then carries out harmlessness disposing.
The main chemical reactions that relates to is following:
(3) electrolysis copper removal
Leachate at first carries out copper removal through electrolysis.Many, the complicated component of metal species in this leachate is according to standard electrode potential E
0(Cu
2+/ Cu)=and 0.3419V, E
0(Ni
2+/ Ni)=-0.257V, electric right electrode potential numerical value is more little, and the reducing power of going back ortho states of material is strong more, and electric right electrode potential numerical value is big more, and the oxidability of the oxidation state of material is strong more.Therefore, the electrolysis of copper is easy to nickel, as long as in electrolytic process, control suitable voltage, just can copper be separated and remove.
Electrolysis copper removal condition is controlled, and can not inject other impurity.Its electrolytic condition is: the pH value of regulating electrolyte is 0.5, and owing to the influence of impurity in the electrolyte, at 2.0～2.5V, temperature is a normal temperature with Control of Voltage, electrolysis time 4h, after the electrolysis in the solution copper ion concentration drop to 4mg/l.The clearance of copper can reach 99.9%.
The key reaction that relates to is following: anode reaction
Anode reaction: 4OH
--4e=2H
2O+O
2
Cathode reaction: 2Cu
2++ 4e=2Cu.
(4) iron impurity
Surplus liquid after the electrolysis adds an amount of sodium chlorate, oxidation 2 hours, sodium chlorate add fashionable, adopt 1% 2, the 2-bipyridyl detects, because Fe
2+With 2, the reaction of 2-bipyridyl can generate sanguine complex ion, when redfree produces, then representes Fe
2+Be oxidized to Oxidation of Fe fully
3+And then the sodium carbonate liquor of adding 90g/l, the pH value of regulator solution is 3.7, can generate ferric hydroxide precipitate this moment, and 85 ℃ of control reaction temperatures, ageing was carried out the press filtration deironing after 1 hour, and filter residue can carry out harmlessness disposing, and the clearance of iron can reach 99.5%.
The key reaction that relates to is following:
ClO
3 -+6Fe
2++6H
+=Cl
-+3H
2O+6Fe
3+；
3CO
3 2-+2Fe
3++3H
2O=2Fe(OH)
3↓+3CO
2↑。
(5) removing calcium and magnesium impurity
The small amount of calcium that contains in the filtrating, magnesium can be removed through adding sodium fluoride.At first in filtrating, add mass concentration and be 30% NaOH solution, regulating pH value of filtrate is 5, adds sodium fluoride again; Adding dose is 3mg/l filtrating, generates calcirm-fluoride and magnesium fluoride deposition, controls 85 ℃ of reaction temperatures equally; After the ageing 2 hours; Remove calcium, magnesium through press filtration, the clearance of calcium magnesium reaches 99.5 %, and filter residue then carries out harmlessness disposing.
The key reaction that relates to is following:
2F
-+Ca
2+=CaF
2↓;
2F
-+Mg
2+=MgF
2↓。
(6) alkaline chemical precipitation
Add mass concentration in the filtrating after removal of impurities and be 30% sodium hydroxide solution, stir, the control pH value of filtrate is 9.5, and precipitation reaction takes place, and ageing was carried out suction filtration after 2 hours, and water repeatedly washes deposition, and the filter cake that obtains is the nickel hydroxide that reclaims out.Generally, the rate of recovery of nickel can reach 98% in this electroplating sludge.Filtrating is then passed through qualified discharge after the wastewater treatment.
The key reaction that relates to is following:
Ni
2++2OH
-=Ni(OH)
2↓。
[0026]Embodiment two: the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise
Shown in accompanying drawing 1, the recycling recovery process of the nickeliferous mud of a kind of electroplating enterprise, form by the following step:
The first step: roasting purifying
With the quality percentage composition of moisture is 72% nickeliferous mud, and roasting obtained the roasting residue in 5 hours under 600～700 ℃ of conditions;
Second step: sulfuric acid leaches
Add water after the roasting residue that at first first step is obtained is pulverized and mix and make mud, under stirring condition, in said mud, add sulfuric acid then, make nickel element and sulfuric acid in the said mud fully react the generation nickelous sulfate, obtain sulphuric leachate; Wherein, said sulfuric acid volume and roasting residue quality ratio between the two are 3:1, and the concentration of said sulfuric acid is 3mol/l;
The 3rd step: filter
With the sulphuric leachate cooling that second step obtained, filter then and obtain filtrating and filter residue; Said residue washing to neutrality is obtained cleaning solution, and this cleaning solution can return the preparation that second step was used for leaching agent sulfuric acid.
The 4th step: electrolysis copper removal
Regulating the 3rd pH value of filtrate to 1 that obtain of step and obtain electrolyte, is the said electrolyte of electrolysis under 2.5 volts the condition at voltage then, makes the concentration of copper ion in this electrolyte be reduced to 3mg/l, obtains the surplus liquid of electrolysis;
The 5th step: iron impurity
In the 4th surplus liquid of electrolysis that obtains of step, add sodium chlorate; Make the abundant oxidation of ferrous ion in the surplus liquid of said electrolysis generate ferric ion; Then under 90 ℃ of conditions; Aqueous sodium carbonate with 80g/l transfers to 3.7 with the pH value, makes said ferric ion generate ferric hydroxide precipitate fully, obtains deironing filtrating after the filtration;
The 6th step: removing calcium and magnesium impurity
Using the quality percentage composition is that the deironing pH value of filtrate that 25% sodium hydrate aqueous solution obtained for the 5th step transfers to 6; Then under 80 ℃ of conditions; Add sodium fluoride, make calcium ion and magnesium ion in the said deironing filtrating generate calcirm-fluoride and magnesium fluoride deposition respectively, obtain removing calcium and magnesium filtrating after the filtration; Wherein, add 10 milligrams of sodium fluorides in the per 1 liter deironing filtrating;
The 7th step: alkaline chemical precipitation
Under stirring condition; Adding quality percentage composition was 25% sodium hydrate aqueous solution during the removing calcium and magnesium that obtains to the 6th step was filtrated; Make that said removing calcium and magnesium pH value of filtrate is 10, make the nickel ion in the said removing calcium and magnesium filtrating generate nickel hydroxide precipitate, the filter cake that obtains after the filtration is nickel hydroxide.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (3)
1. the recycling recovery process of the nickeliferous mud of electroplating enterprise is characterized in that: mainly be made up of the following step:
The first step: roasting purifying
With the quality percentage composition of moisture is 70～75% nickeliferous mud, and roasting obtained the roasting residue in 5～6 hours under 600～700 ℃ of conditions;
Second step: sulfuric acid leaches
Add water after the roasting residue that at first first step is obtained is pulverized and mix and make mud, under stirring condition, in said mud, add sulfuric acid then, make nickel element and sulfuric acid in the said mud fully react the generation nickelous sulfate, obtain sulphuric leachate; Wherein, said sulfuric acid with roasting residue mixed proportion between the two is: per 2～3 milliliters of sulfuric acid mix with 1 gram roasting residue; The concentration of said sulfuric acid is 3～4mol/l;
The 3rd step: filter
With the sulphuric leachate cooling that second step obtained, filter then and obtain filtrating and filter residue;
The 4th step: electrolysis copper removal
Obtaining electrolyte below regulating the 3rd pH value of filtrate to 1 or 1 that obtain of step, is the said electrolyte of electrolysis under 2～2.5 volts the condition at voltage then, and the concentration of copper ion in this electrolyte is reduced to below the 5mg/l, obtains the surplus liquid of electrolysis;
The 5th step: iron impurity
In the 4th surplus liquid of electrolysis that obtains of step, add sodium chlorate; Make the abundant oxidation of ferrous ion in the surplus liquid of said electrolysis generate ferric ion; Then under 80～90 ℃ of conditions; The pH value is transferred to 3.9～4.1, make said ferric ion generate ferric hydroxide precipitate fully, obtain deironing filtrating after the filtration;
The 6th step: removing calcium and magnesium impurity
The deironing pH value of filtrate that the 5th step was obtained transfers to 4.5～6, under 80～90 ℃ of conditions, adds sodium fluoride then, makes calcium ion and magnesium ion in the said deironing filtrating generate calcirm-fluoride and magnesium fluoride deposition respectively, obtains removing calcium and magnesium filtrating after the filtration; Wherein, add 1～10g sodium fluoride in every liter of deironing filtrating;
The 7th step: alkaline chemical precipitation
Under stirring condition; Adding quality percentage composition was 25～35% sodium hydrate aqueous solution during the removing calcium and magnesium that obtains to the 6th step was filtrated; Make that said removing calcium and magnesium pH value of filtrate is 9～10; Make the nickel ion in the said removing calcium and magnesium filtrating generate nickel hydroxide precipitate, the filter cake that obtains after the filtration is nickel hydroxide.
2. the recycling recovery process of the nickeliferous mud of electroplating enterprise according to claim 1 is characterized in that: residue washing to the neutrality that said the 3rd step is obtained obtains cleaning solution, and this cleaning solution can be back to the preparation that is used to leach reagent of sulfuric acid in second step.
3. the recycling recovery process of the nickeliferous mud of electroplating enterprise according to claim 1 is characterized in that: in said the 6th step, using the quality percentage composition is that 25～35% sodium hydrate aqueous solution transfers to 4.5～6 with the pH value.
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| CN102786134A (en) * | 2012-08-07 | 2012-11-21 | 华南理工大学 | Method for removing iron from acid waste etching solution of printed circuit boards |
| CN103241758B (en) * | 2013-05-17 | 2016-11-23 | 崔岷 | The method that the bed mud produced with fluoride waste produces calcium fluoride |
| CN103979755A (en) * | 2014-05-27 | 2014-08-13 | 昆山市益民环保技术开发有限公司 | Comprehensive treatment method of electro-plating sludge and sludge containing low amount of copper |
| CN105256141B (en) * | 2015-10-26 | 2017-12-19 | 广西银亿再生资源有限公司 | A kind of electric plating sludge resource processing and the method for comprehensive reutilization |
| CN106282573B (en) * | 2016-08-24 | 2018-11-30 | 盛隆资源再生（无锡）有限公司 | A method of recycling metal resource from hazardous solid waste |
| CN106636654B (en) * | 2016-12-31 | 2019-04-26 | 山东飞源科技有限公司 | The method of metallic nickel is recycled from fluorine-containing electrolysis fused salt |
| CN107265798A (en) * | 2017-06-29 | 2017-10-20 | 山东毅康科技股份有限公司 | A kind of method for sludge treatment |
| CN109593966A (en) * | 2018-12-27 | 2019-04-09 | 山东飞源科技有限公司 | The process of smart nickel is extracted in plating from Nitrogen trifluoride nickel slag |
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| CN110983070B (en) * | 2019-11-29 | 2020-12-15 | 长沙华时捷环保科技发展股份有限公司 | Method for preparing refined nickel sulfate from copper electrolyte decoppered liquid |
| CN111302576A (en) * | 2019-12-13 | 2020-06-19 | 泰州明锋资源再生科技有限公司 | Harmless treatment method for pickling iron-containing sludge |
| CN112718794B (en) * | 2020-12-14 | 2021-11-16 | 深圳市卓域环保科技有限公司 | Harmless muck treatment system |
| CN112981114A (en) * | 2021-02-18 | 2021-06-18 | 甘肃万众环保科技有限公司 | Nickel-containing waste battery and nickel-containing waste residue recovery process |
| CN113322382B (en) * | 2021-08-04 | 2021-11-30 | 清大国华环境集团股份有限公司 | Treatment method for recovering nickel from nickel-containing sludge |
| CN116462245A (en) * | 2023-03-27 | 2023-07-21 | 厦门资生环保科技有限公司 | Sodium washing process method for preparing battery nickel sulfate solution by using high-nickel sludge |
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| JPS5344440A (en) * | 1976-10-05 | 1978-04-21 | Kurita Water Ind Ltd | Treatment process for aluminum surface treating solution |
| JPH10180266A (en) * | 1996-12-27 | 1998-07-07 | Yamato Denki Kogyo Kk | Treatment of waste liquid of electroless nickel plating |
| JP4405281B2 (en) * | 2004-02-18 | 2010-01-27 | 株式会社アステック入江 | Recycling method of electroless nickel plating waste liquid |
| CN101157509A (en) * | 2007-09-04 | 2008-04-09 | 南京南大表面和界面化学工程技术研究中心有限责任公司 | Electroplating wastewater zero-discharge or low-discharge handling method |
| CN101786775A (en) * | 2010-02-10 | 2010-07-28 | 中南大学 | Method for selective recovery of copper and nickel from electroplating sludge |
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