CN102618882B - Electrolysis recovery method of nickel in waste water - Google Patents
Electrolysis recovery method of nickel in waste water Download PDFInfo
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Abstract
Disclosed is an electrolysis recovery method of nickel in waste water. The method includes steps of: firstly, selecting 1000-1500 parts of waste water containing nickel, using sodium hydroxide flakes to regulate PH in a range of 1-6; secondly, adding 0.01-0.05 parts of polyethylene glycol, 0.03-0.06 parts of thiourea, 0.01-0.015 parts of at least one of sodium dodecyl sulfate, chloral hydrate, para toluene sulfonamide and saccharin, maintaining a system temperature at 50-80 DEG C, controlling current to in a range of 1.0-5.0A and starting electrolysis with stirring, maintaining the PH the same as that in the first step through adding the sodium hydroxide flakes, and controlling electrolysis time in a range of 12-24 hours; and thirdly, using sodium hydroxide flakes again to regulate the PH in a range of 6-10, adding 0.15-0.3 parts of at least one of sodium monophosphate and gelatin, maintaining the system temperature continuously, controlling current to in a range of 1.0-5.0A and starting electrolysis with stirring, and controlling electrolysis time in a range of 8-16 hours. The electrolysis recovery method of the nickel in the waste water is high in applicability, simple and convenient, low in cost; and can obtain metallic nickel directly.
Description
Technical field
The present invention relates to the metal recovery technical field in waste water, especially relate to the technique that in a kind of waste water, nickel reclaims.
Background technology
Along with the fast development of national economy, and the improving constantly of people's living condition, the requirement of the electronics products such as household electrical appliance, Cell phone, video player is also increasing, and the demand of one of its core component wiring board is also to grow with each passing day thereupon.But because wiring board industry can produce a large amount of heavy metal wastewater therebies in process of production, effective disposal of these heavy metal wastewater therebies just becomes a great problem of pendulum in face of Economic development.Nickel-containing waste water is as one of main waste water of wiring board industry, annual millions of ton of meter of generation, and nickel contamination can cause dermatitis and trachitis, even there is pneumonia, nickel has the effect of accumulating, and accumulates at most in kidney,spleen,liver, can bring out a series of serious diseases such as nasopharyngeal carcinoma and lung cancer.And nickel is as a kind of precious metal, its price is very expensive.Therefore, in nickel-containing waste water, the recovery method of nickel seems particularly important, extremely has economy and social value.
The nickel-containing waste water that wiring board industry produces is mainly chemical nickel plating and two kinds of operations of electronickelling produce, nickel in the waste water that wherein chemical nickel plating produces mainly exists with complex status, nickel in the waste water that electronickelling produces mainly exists with ionic condition, but also some exists with complex status.Just make like this when reclaiming nickel difficulty very, because this just relates to a series of difficult problems such as contact break, condition control.
The domestic research for this part is at present also more, but most recovery method is just just for a kind of waste water wherein, simpler for some treatment process of electronickelling waste water, and the also primary products of nickel salt and so on just that arrive, as adopting to press filtration after hydro-oxidation sodium in electronickelling waste water, Shao Lin obtains nickel salt; Some treatment process can utilize electronickelling waste water to obtain metallic nickel, but that complex steps, operational condition require is high, as Shanghai company limited of light industry institute by reverse osmosis or ion selective membrane concentrating spent liquor after, re-use three-dimensional electrolysis equipment and obtain metallic nickel.For chemical nickle-plating wastewater, Feng Yunxiang adopts strongly basic anion exchange resin to process nickel-plating waste water, makes complexing nickel de-steady, then with contained nickel ion in storng-acid cation exchange resin absorption nickel-plating waste water; Mitac Precision Technology (Kunshan) Corp. adopts sodium hypophosphite and Palladous chloride under heating condition, to take nickel plate and obtains metallic nickel as substrate decomposes.Sum up these methods and can find not only complicated operation, with high costs, but also just for a certain nickel-containing waste water, and the nickeliferous waste liquid that a lot of Electronics Factories discharge is the mixed waste liquor of the two, therefore, one can directly be reclaimed seem especially important of nickel-containing waste water and method convenient and swift, with low cost.
The recovery of nickel-containing waste water mainly contains following 3 difficulties: first, in nickel-containing waste water, the content of nickel is generally not high, and existence form differs, have ionic condition, also has complex status, and treatment process is all different, and processing cost is higher; Secondly, impurity component complexity and content are high, as the unusual height all of phosphorus, ammonia-nitrogen content in chemical nickeling ageing liquid, and also unusual height of chlorion, boric acid content in electronickelling waste water, the existence of these impurity components makes the recycling of nickel in waste liquid very difficult; Again, it is stable that nickel-containing waste water water quality can not keep, the method that this just need to process according to reality judgement and the consumption of medicament.
Summary of the invention
The problems referred to above that exist for prior art, the applicant provides the electrolytic recovery method of nickel in a kind of waste water.Method applicability provided by the present invention is strong, can directly obtain metallic nickel, and method is easy, with low cost.
Technical scheme of the present invention is as follows:
An electrolytic recovery method for nickel in waste water, concrete steps are as follows:
(1) get 1000 parts to 1500 parts nickel-containing waste waters, with flaky sodium hydrate, regulate pH in 1 ~ 6 scope;
(2) add at least one in 0.01 part to 0.05 part polyoxyethylene glycol, 0.03 part to 0.06 part thiocarbamide, 0.01 part to 0.015 part sodium laurylsulfonate, chloral hydrate, para toluene sulfonamide or asccharin, maintenance system temperature is at 50 ~ 80 ℃, stir lower control electric current and within the scope of 1.0 ~ 5.0A, start electrolysis, and by adding flaky sodium hydrate to keep system pH identical with step (1), electrolysis time is controlled at 12 ~ 24h;
(3) and then with flaky sodium hydrate regulation system pH in 6 ~ 10 scopes, add at least one in 0.15 part to 0.3 part inferior sodium phosphate or gelatin, continue to keep system temperature, stir the electrolysis within the scope of 1.0 ~ 5.0A of lower control electric current, electrolysis time is 8 ~ 16h.
During electrolysis, take titanium plate as negative plate, and titanium plating iridium plate is that in positive plate control step (2), stirring velocity is 700 ~ 900 r/min, and in step (3), stirring velocity is 900 ~ 1100 r/min.
The technique effect that the present invention is useful is:
The present invention compare with existing method have advantages of following outstanding: first, the method is applicable to the recovery of all nickel-containing waste waters, and is not only confined to a certain nickel-containing waste water; Secondly, by the method, reclaiming what obtain is the nickel of metallic state, rather than nickel salt and so on also need further to process the product that could use, meet environmental protection theory; Again, whole process energy consumption is very low, has realized less energy-consumption, low-cost recovery; Finally, by this method, reclaim the nickel purity obtaining higher, and be very easy to remove from negative plate easy handling.This invention has the reason of above several advantages to have:
(1) for low this problem of electrolytic recovery that is difficult for of content of nickel in nickel-containing waste water, first, by controlling Faradaic current electrolysis within the scope of 1.0 ~ 5.0A, make full use of Faradaic current, reduce energy consumption, reduce the generation of side reaction; Secondly, with polyoxyethylene glycol, increase cathodic polarization efficiency, realize the good wet effect of anticathode plate, the gas producing in electrolysis is overflowed fast, guarantee that the nickel obtaining is smooth; Again, with thiocarbamide, increase the nucleation density of electrolytic nickel, reduce cathodic current, improve electrolytic efficiency; The more important thing is, adding of one or more in sodium laurylsulfonate, chloral hydrate, para toluene sulfonamide, asccharin, reduced on the one hand the internal stress of nickel dam, make nickel dam uniform and delicate and there is metalluster, accelerated on the other hand the effusion of the hydrogen of negative electrode generation, prevent the local alkalization of negative plate that the change in concentration because of nickel in waste liquid causes, generate nickel hydroxide precipitate Pollution System, affect further carrying out of electrolytic process.
(2) for high this problem of chloride ion content in waste liquid, first by hierarchy of control temperature, within the scope of 50 ~ 80 ℃, carry out electrolysis, the chlorine producing on positive plate is overflowed fast, avoid generating hypochlorite because chlorine is dissolved in system on the one hand, the hypochlorite of generation can react with nickel ion the NiO that obtains black
2nH
2o, stops further carrying out of electrolysis, improves on the other hand current efficiency, reduces the generation of electrolysis side reaction, prevents from damaging positive plate; Secondly, electrolysis is carried out under rapid stirring, guaranteed that on the one hand chlorine overflows fast, also make on the other hand the nickel in system be evenly distributed, the Faradaic current utilizing to greatest extent; Again, due to the competition electric discharge of chlorion on positive plate, make the pH value of system constantly increase, after surpassing certain limitation, can generate nickel hydroxide precipitate, affecting electrolysis carries out, therefore in electrolytic process, need the pH of the system of keeping a close eye on to change, the electrolysis first stage, strict hierarchy of control pH was in 1 ~ 6 scope.
Embodiment
embodiment 1
(1) get 1000 g nickel-containing waste waters, with flaky sodium hydrate, regulating pH value is 2.0;
(2) add 0.01g polyoxyethylene glycol, 0.03g thiocarbamide, 0.005g sodium laurylsulfonate and 0.005g asccharin, maintenance system temperature is at 70 ℃, and it is that 1.0 A start electrolysis that 700 r/min stir lower control electric current, surveys the pH value of a system per half an hour, by adding flaky sodium hydrate maintenance system pH, be 2.0, electrolysis time is controlled at 12 h, take titanium plate as negative plate during electrolysis, and titanium plating iridium plate is positive plate;
And then be 6.0 by flaky sodium hydrate regulation system pH value (3), add 0.1g inferior sodium phosphate and 0.05g gelatin, continue to keep system temperature, 900 r/min stir lower control electric current in 1.0 A electrolysis, electrolysis time is 8 h, take titanium plate as negative plate during electrolysis, and titanium plating iridium plate is positive plate.The results are shown in Table shown in 1.
embodiment 2
(1) get 1300 g nickel-containing waste waters, with flaky sodium hydrate, regulating pH value is 3.0;
(2) add 0.04 g polyoxyethylene glycol, 0.05 g thiocarbamide, 0.01g chloral hydrate and 0.005g asccharin, maintenance system temperature is at 50 ℃, and 800 r/min stir lower control electric current and start electrolysis at 3.0A, survey the pH value of a system per half an hour, by adding flaky sodium hydrate maintenance system pH, be 3.0, electrolysis time is controlled at 20 h, take titanium plate as negative plate during electrolysis, and titanium plating iridium plate is positive plate;
And then be 9.0 by flaky sodium hydrate regulation system pH value (3), add 0.2g inferior sodium phosphate, continue to keep system temperature, 1000 r/min stir lower control electric current in 2.5 A electrolysis, electrolysis time is 10 h, take titanium plate as negative plate during electrolysis, and titanium plating iridium plate is positive plate.The results are shown in Table shown in 1.
embodiment 3
(1) get 1500 g nickel-containing waste waters, with flaky sodium hydrate, regulating pH value is 5.5;
(2) add 0.05 g polyoxyethylene glycol, 0.06 g thiocarbamide, 0.007g para toluene sulfonamide and 0.005g asccharin, maintenance system temperature is at 80 ℃, and 900 r/min stir lower control electric current and start electrolysis at 5.0 A, survey the pH value of a system per half an hour, by adding flaky sodium hydrate maintenance system pH, be 5.5, electrolysis time is controlled at 24 h, take titanium plate as negative plate during electrolysis, and titanium plating iridium plate is positive plate;
And then be 10.0 by flaky sodium hydrate regulation system pH value (3), add 0.15g inferior sodium phosphate and 0.15g gelatin, continue to keep system temperature, 1100 r/min stir lower control electric current in 5.0 A electrolysis, electrolysis time is 16 h, during electrolysis, take titanium plate as negative plate, and titanium plating iridium plate is positive plate.The results are shown in Table shown in 1.
The contrast of nickel content in nickel-containing waste water before and after table 1 electrolysis
By table 1, we can clearly be seen that: the method is very effective for the nickel reclaiming in nickel-containing waste water, the nickel-containing waste water of processing by the method, and the rate of recovery of nickel can reach more than 98%.Contrast the method and existing method, method of the present invention not only suitability is wide, and technique is relatively simple, with low cost, more can directly obtain the nickel of metallic state, and economy, social value are all very high, are worthy of further application very much.
Claims (3)
1. an electrolytic recovery method for nickel in electronickelling waste water, is characterized in that concrete steps are as follows:
(1) get 1000 parts to 1500 parts nickel-containing waste waters, with flaky sodium hydrate, regulate pH in 1 ~ 6 scope;
(2) add at least one in 0.01 part to 0.05 part polyoxyethylene glycol, 0.03 part to 0.06 part thiocarbamide, 0.01 part to 0.015 part sodium laurylsulfonate, chloral hydrate, para toluene sulfonamide or asccharin, maintenance system temperature is at 50 ~ 80 ℃, stir lower control electric current and within the scope of 1.0 ~ 5.0A, start electrolysis, and by adding flaky sodium hydrate to keep system pH identical with step (1), electrolysis time is controlled at 12 ~ 24h;
(3) and then with flaky sodium hydrate regulation system pH in 6 ~ 10 scopes, add at least one in 0.15 part to 0.3 part inferior sodium phosphate or gelatin, continue to keep system temperature, stir the electrolysis within the scope of 1.0 ~ 5.0A of lower control electric current, electrolysis time is 8 ~ 16h;
Described nickel-containing waste water is electronickelling waste water.
2. the electrolytic recovery method of nickel in electronickelling waste water according to claim 1, take titanium plate as negative plate while it is characterized in that electrolysis, and titanium plating iridium plate is positive plate.
3. the electrolytic recovery method of nickel in electronickelling waste water according to claim 1, it is characterized in that controlling stirring velocity in step (2) is 700 ~ 900 r/min, in step (3), stirring velocity is 900 ~ 1100 r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3211983B2 (en) * | 1992-07-14 | 2001-09-25 | 船井電機株式会社 | Notification method of replacement time of electrolytic electrode of ion water generator |
| JP2001353489A (en) * | 2000-06-14 | 2001-12-25 | Babcock Hitachi Kk | Nh3-containing waste water treatment device and treatment method |
| CN102212842A (en) * | 2011-05-26 | 2011-10-12 | 无锡中天固废处置有限公司 | Method for recovering nickel in chemical nickel-plating ageing liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100532656C (en) * | 2005-12-19 | 2009-08-26 | 赵小毛 | Method for recovering copper and nickel nitrate by electrolysis of electroplating waste water |
| CN100594265C (en) * | 2007-03-12 | 2010-03-17 | 张建玲 | Method for producing electrolytic nickel by using various nickel-containing raw materials |
| CN102162036B (en) * | 2011-04-08 | 2012-09-26 | 湖州金泰科技股份有限公司 | Process for enriching copper and nickel in electroplating copper-nickel mixed waste water |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3211983B2 (en) * | 1992-07-14 | 2001-09-25 | 船井電機株式会社 | Notification method of replacement time of electrolytic electrode of ion water generator |
| JP2001353489A (en) * | 2000-06-14 | 2001-12-25 | Babcock Hitachi Kk | Nh3-containing waste water treatment device and treatment method |
| JP3984414B2 (en) * | 2000-06-14 | 2007-10-03 | バブコック日立株式会社 | NH3-containing wastewater treatment apparatus and treatment method |
| CN102212842A (en) * | 2011-05-26 | 2011-10-12 | 无锡中天固废处置有限公司 | Method for recovering nickel in chemical nickel-plating ageing liquid |
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