CN101058436A - Circuit board and electric plating sludge resource recovery process - Google Patents
Circuit board and electric plating sludge resource recovery process Download PDFInfo
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- CN101058436A CN101058436A CN 200610079217 CN200610079217A CN101058436A CN 101058436 A CN101058436 A CN 101058436A CN 200610079217 CN200610079217 CN 200610079217 CN 200610079217 A CN200610079217 A CN 200610079217A CN 101058436 A CN101058436 A CN 101058436A
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Abstract
The invention discloses a circuit board and resouring recycling technique of plated sludge, which is characterized by the following: leaching the sludge through dilute sulfuric acid; controlling Na2S and pH value to sediment zinc and nickel; recycling chromium iron through liquid alkaline sediment; using iron chips to replace and recycle copper; solidifying the leached tail slag as building material with reliable technique; separating and extracting zinc and nickel effectively; improving the utility of zinc and nickel resource; reducing the discharge of waste; realizing environmental protection.
Description
Technical field
The present invention relates to the recycling recovery process of a kind of IT circuit card and electroplating sludge, relate in particular to the recovery technology of a kind of nickel, zinc.
Background technology
" non-ferrous metals industry " (2000 the 12nd phase 45-47 pages or leaves) is disclosed: " extracting the experimental study of copper and single nickel salt from electroplating sludge ", its technological process mainly comprises leaching, replaces, purifies, produces single nickel salt and solidification treatment 5 parts.The employing dilute sulphuric acid leaches, iron powder replacement.The scavenging process proceed step by step; The first step adds an amount of Na
2S; Second step added sodium chlorate, sodium carbonate solution control pH value; The 3rd goes on foot with the adjustment of NaOH solution, adds an amount of NaF, filters isolation of purified liquid and purification slag at last.Add an amount of Na in the scavenging process
2S can remove zine ion and the cupric ion in the solution, and almost not loss of nickel, in second step of scavenging process, the chromium in the solution generates precipitation.Single nickel salt evaporates and crystallization, obtains the single nickel salt of industrial primary standard, and the rate of recovery of nickel is greater than 80%.Leached mud solidifies with the purification slag.Adopt this technological process can only obtain single nickel salt, and the subject range relative narrower of single nickel salt.
Summary of the invention
The present invention aims to provide the recovery technology of a kind of circuit card and electric plating sludge resource, by this technological process, with the copper in circuit card and the electroplating sludge, zinc, nickel, chromium, these metals resourcesization of iron, the realization regeneration is worth, thereby solve pollution problem, make the resource utilization of nickel, zinc can satisfy purposes needs more widely environment.
To achieve these goals, circuit card of the present invention and electric plating sludge resource recovery process are: 1) leach: add dilution heat of sulfuric acid in circuit card and electroplating sludge, leach at normal temperatures, Gu circuit card and electroplating sludge liquid H
2SO
4Than being 1: 0.6, leaching terminal point control pH value is 1.5-2, and extraction time is 40 minutes; 2) displacement: through leaching after-filtration, in filtrate, add iron filings under the normal temperature with displacement copper, the iron filings add-on is 1.4 times of filtrate copper content, stirred 30 minutes, filter then, cupric 70%-90% copper sponge is added coke, lime, sand in proportion, insert blast furnace and slightly refine, make cupric greater than 95% copper bullion; 3) zinc sulphide precipitation: at normal temperatures, adjust the pH value of filtrate, the pH value that makes filtrate is 1.5-3, presses Zn: Na then
2S=1: 2 ratio adds 30%Na
2S solution stirred 1 hour, filtered again, made to contain zinc greater than 50% zinc sulphide; 4) nickel sulphide precipitation: at normal temperatures, adjust the pH value of filtrate, the pH value that makes filtrate is 3-5, and then in nickel: the ratio of sodium sulphite=1: 2 slowly adds 30%Na
2S solution stirred 40 minutes, through filtering, made nickeliferous greater than 30% nickelous sulfide; 5) chromium iron precipitation: at normal temperatures, add 30%NaOH solution in filtrate, the pH value of control filtrate is 9-10, stirred 10 minutes, and refiltered, make ferrochrome oxyhydroxide, it is inserted 670-690 ℃ of following roasting, make the mixed oxide that contains chromic oxide 60%, ferric oxide 30%.6) leaching tailings solidifies: leaching tailings mainly is CaSO
4, sand, copper, zinc, nickel, chromium, iron is all less than 0.2%, by leached mud: cement: sand is that 1: 2.5: 1 mixed is even, places mould to leave standstill and makes its curing in 24 hours.
In leaching at normal temperatures with dilute sulphuric acid and mud, because in and in the mud metal compound attitude be oxyhydroxide, the therefore very easy leach liquor that enters of most metal ions, leaching terminal point control pH value is 1.5-2, the low excessively copper that is unfavorable for of pH value is replaced, and pH value is too high can to influence metal leaching rate.
During with iron powder replacement copper, in the displacement slot outlet screen cloth is set, the crude iron bits can not pump with copper sponge, so the grade of copper sponge is higher, can save the consumption of iron simultaneously, and unreacted iron can continue to use.
Use Na
2S makes in the sedimentary process of zinc sulphide, must strictly control PH at 1.5-3, and zinc sulphide almost completely precipitates like this, if pH value is too high, the precipitation of iron is increased, and influence the grade of zinc.
Use Na
2S makes in the nickel sulphide precipitation process, also must strictly control PH at 3-5, if pH value is too high, the precipitation of iron is increased, and influence the grade of nickel.
Adopt Technology of the present invention to handle electroplating sludge and circuit card, available copper grade is greater than 95%, and the rate of recovery is greater than 94%; The nickel grade is greater than 30%, and the rate of recovery is greater than 90%; The zinc grade is greater than 50%, and the rate of recovery is greater than 90%; In the ferrochrome oxide compound chromium greater than 60%, iron is greater than 30%, meets the requirement of making the ferrochrome raw material, realized that comprehensive recovery of gold belongs to the purpose of resource.
Adopt Technology of the present invention to handle the tailings that the electroplating sludge circuit card is produced, after solidification treatment, its metallic salt can be with the water environment of transferring the pollution, the waste water 80% that technology produces recycles, 20% treatedly effluxes after up to standard, has fundamentally solved and has handled the influence that mud causes environment.
Adopt the prepared zinc sulphide of Technology of the present invention, nickelous sulfide, its range of application is more extensive, has overcome the deficiency that single nickel salt is of limited application.
Description of drawings
Fig. 1 is a technological process block-diagram of the present invention.
Embodiment
Shown in Figure 1, mud is inserted leaching vat, be 1: 0.6 ratio in solid-to-liquid ratio, add dilute sulphuric acid, stirred at normal temperatures 40 minutes, the pH value of control terminal point leach liquor is 1.5-2, filters then, filtrate is pumped into displacement slot, the leached mud otherwise processed; In the filtrate of displacement slot, extraordinarily go into iron filings by 1.4 of filtrate copper content, stirred at normal temperatures 30 minutes, filter then, filtrate pumping into carried the zinc groove, obtain the copper sponge of cupric 70-90% simultaneously, copper sponge is added coke, lime, sand in proportion, insert blast furnace after mixing thoroughly in the lump and slightly refine, make cupric greater than 95% copper bullion; Add NaOH the filtrate of carrying the zinc groove, the pH value of control filtrate is 1.5-3, compares Na by zinc
2S is that 1: 2 ratio adds 30%Na
2S solution stirs 1 hour (60 minutes) at normal temperatures, filters then, and filtrate pumping into carried the nickel groove, obtain simultaneously to contain zinc greater than 50% at zinc sulphide; The pH value that filtrate in the nickel groove is carried in control is 3-5, compares Na by nickel
2S is that 1: 2 ratio slowly adds 30%Na
2S solution stirred 40 minutes at normal temperatures, filtered then, and filtrate is pumped into settling bath, obtained nickeliferous greater than 30% nickelous sulfide simultaneously; Add 30%NaOH in the filtrate in settling bath, the PH of control filtrate is 9-10, stirs at normal temperatures 10 minutes, filter then, make ferrochrome oxyhydroxide, again ferrochrome oxyhydroxide is placed 670 ° of-690 ℃ of following roastings, obtain to contain the mixed oxide of chromic oxide 60%, ferric oxide 30%; The filtrate of this moment is waste water, and it 80% returns leaching vat and continue to use, and 20% send pyrogenic process to make water coolant; Leached mud mainly is CaSO
4, sand, in leached mud: cement: sand is that 1: 2.5: 1 ratio stirs evenly, and the pattern tool of placing leaves standstill and made its curing in 24 hours, as material of construction.
Claims (6)
1, a kind of circuit card and electric plating sludge resource recovery process by leaching, displacement, precipitation, curing process proceed step by step, is characterized in that at normal temperatures, and the pH value of regulating the filtrate after replacing is 1.5-3, compares Na by zinc
2S is that 1: 2 ratio adds 30%Na
2S solution stirred 60 minutes, made after filtration to contain zinc greater than 50% zinc sulphide; Regulating the pH value carry the filtrate behind the zinc then is 3-5, compares Na by nickel
2S is that 1: 2 ratio slowly adds 30%Na
2S solution stirred 40 minutes, made nickeliferous greater than 30% nickelous sulfide after filtration.
2, circuit card according to claim 1 and electric plating sludge resource recovery process, the pH value that it is characterized in that regulating metathetical filtrate is 2.
3, circuit card according to claim 1 and electric plating sludge resource recovery process, the pH value that it is characterized in that regulating metathetical filtrate is 2.5.
4, circuit card according to claim 1 and electric plating sludge resource recovery process, it is characterized in that regulating the pH value of carrying the filtrate behind the zinc is 3.5.
5, circuit card according to claim 1 and electric plating sludge resource recovery process, it is characterized in that regulating the pH value of carrying the filtrate behind the zinc is 4.
6, circuit card according to claim 1 and electric plating sludge resource recovery process, it is characterized in that regulating the pH value of carrying the filtrate behind the zinc is 4.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100792171A CN100532271C (en) | 2006-04-17 | 2006-04-17 | Circuit board and electric plating sludge resource recovery process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100792171A CN100532271C (en) | 2006-04-17 | 2006-04-17 | Circuit board and electric plating sludge resource recovery process |
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| Publication Number | Publication Date |
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| CN101058436A true CN101058436A (en) | 2007-10-24 |
| CN100532271C CN100532271C (en) | 2009-08-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100792171A Expired - Fee Related CN100532271C (en) | 2006-04-17 | 2006-04-17 | Circuit board and electric plating sludge resource recovery process |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643243A (en) * | 2009-08-14 | 2010-02-10 | 扬州宁达贵金属有限公司 | Method for recycling copper, nickel, chromium, zinc and iron from plating sludge |
| CN102303940A (en) * | 2011-08-22 | 2012-01-04 | 陕西科技大学 | Method for treating sludge containing trivalent chromium |
| CN101921918B (en) * | 2010-02-05 | 2012-01-04 | 吕忠庆 | Method for recovering metals and plastics from waste plastics containing metal plated layers |
| CN102417987A (en) * | 2011-08-09 | 2012-04-18 | 朱小红 | Method for recovering valuable metal from electroplating sludge |
| CN102557299A (en) * | 2012-01-11 | 2012-07-11 | 浙江海拓环境技术有限公司 | Recovery method of copper-nickel heavy metals in electroplated mixed-flow waste water |
| CN102557297A (en) * | 2011-12-31 | 2012-07-11 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN103221557A (en) * | 2011-11-22 | 2013-07-24 | 住友金属矿山株式会社 | Method for producing nickel-ontaining acidic solution |
| CN103372563A (en) * | 2012-04-20 | 2013-10-30 | 连云港荣鼎金属有限公司 | Waste treatment method |
| CN106756034A (en) * | 2016-12-05 | 2017-05-31 | 昆明理工大学 | A kind of method of the step of composite waste containing chromium Recovery Purifying valuable metal |
| CN110616328A (en) * | 2019-09-29 | 2019-12-27 | 江苏艾信环境工程有限公司 | Method for preparing iron-chromium black from chromium-containing electroplating sludge |
| CN111304444A (en) * | 2020-03-26 | 2020-06-19 | 无锡中天固废处置有限公司 | Treatment method for separating and recovering copper, iron, zinc, nickel and chromium from chromium-containing sludge |
| CN113322382A (en) * | 2021-08-04 | 2021-08-31 | 清大国华环境集团股份有限公司 | Treatment method for recovering nickel from nickel-containing sludge |
-
2006
- 2006-04-17 CN CNB2006100792171A patent/CN100532271C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643243A (en) * | 2009-08-14 | 2010-02-10 | 扬州宁达贵金属有限公司 | Method for recycling copper, nickel, chromium, zinc and iron from plating sludge |
| CN101643243B (en) * | 2009-08-14 | 2014-01-15 | 扬州宁达贵金属有限公司 | Method for recycling copper, nickel, chromium, zinc and iron from plating sludge |
| CN101921918B (en) * | 2010-02-05 | 2012-01-04 | 吕忠庆 | Method for recovering metals and plastics from waste plastics containing metal plated layers |
| CN102417987A (en) * | 2011-08-09 | 2012-04-18 | 朱小红 | Method for recovering valuable metal from electroplating sludge |
| CN102303940A (en) * | 2011-08-22 | 2012-01-04 | 陕西科技大学 | Method for treating sludge containing trivalent chromium |
| CN102303940B (en) * | 2011-08-22 | 2013-06-05 | 陕西科技大学 | Method for treating sludge containing trivalent chromium |
| CN103221557A (en) * | 2011-11-22 | 2013-07-24 | 住友金属矿山株式会社 | Method for producing nickel-ontaining acidic solution |
| CN102557297B (en) * | 2011-12-31 | 2013-10-02 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN102557297A (en) * | 2011-12-31 | 2012-07-11 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN102557299A (en) * | 2012-01-11 | 2012-07-11 | 浙江海拓环境技术有限公司 | Recovery method of copper-nickel heavy metals in electroplated mixed-flow waste water |
| CN102557299B (en) * | 2012-01-11 | 2013-06-12 | 浙江海拓环境技术有限公司 | Recovery method of copper-nickel heavy metals in electroplated mixed-flow waste water |
| CN103372563A (en) * | 2012-04-20 | 2013-10-30 | 连云港荣鼎金属有限公司 | Waste treatment method |
| CN106756034A (en) * | 2016-12-05 | 2017-05-31 | 昆明理工大学 | A kind of method of the step of composite waste containing chromium Recovery Purifying valuable metal |
| CN110616328A (en) * | 2019-09-29 | 2019-12-27 | 江苏艾信环境工程有限公司 | Method for preparing iron-chromium black from chromium-containing electroplating sludge |
| CN111304444A (en) * | 2020-03-26 | 2020-06-19 | 无锡中天固废处置有限公司 | Treatment method for separating and recovering copper, iron, zinc, nickel and chromium from chromium-containing sludge |
| CN111304444B (en) * | 2020-03-26 | 2021-08-24 | 无锡中天固废处置有限公司 | Treatment method for separating and recovering copper, iron, zinc, nickel and chromium from chromium-containing sludge |
| CN113322382A (en) * | 2021-08-04 | 2021-08-31 | 清大国华环境集团股份有限公司 | Treatment method for recovering nickel from nickel-containing sludge |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100532271C (en) | 2009-08-26 |
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Granted publication date: 20090826 Termination date: 20140417 |